 
data_22-0902
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C18 H28 Br4 N2 Pb' 
_chemical_formula_weight          799.22

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Br'  'Br'  -0.6763   1.2805
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pb'  'Pb'  -4.0753   8.5060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    18.2507(4)
_cell_length_b                    7.8185(2)
_cell_length_c                    8.4334(2)
_cell_angle_alpha                 90
_cell_angle_beta                  94.822(2)
_cell_angle_gamma                 90
_cell_volume                      1199.13(5)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     673
_cell_measurement_theta_min       4.9060
_cell_measurement_theta_max       29.0640
 
_exptl_crystal_description        block
_exptl_crystal_colour             white
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     2.214          
_exptl_crystal_F_000              744
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_absorpt_coefficient_mu     21.513
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      1.54184
_diffrn_radiation_type            CuK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             7554
_diffrn_reflns_av_unetI/netI      0.0719
_diffrn_reflns_av_R_equivalents   0.1278
_diffrn_reflns_limit_h_min        -21
_diffrn_reflns_limit_h_max        22
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        8
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          4.863
_diffrn_reflns_theta_max          75.924
_diffrn_reflns_theta_full         67.684
_diffrn_measured_fraction_theta_max   0.972
_diffrn_measured_fraction_theta_full  0.993
_diffrn_reflns_Laue_measured_fraction_max    0.972
_diffrn_reflns_Laue_measured_fraction_full   0.993
_diffrn_reflns_point_group_measured_fraction_max   0.972
_diffrn_reflns_point_group_measured_fraction_full  0.993
_reflns_number_total              2436
_reflns_number_gt                 2368
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          2436
_refine_ls_number_parameters      117
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0983
_refine_ls_R_factor_gt            0.0968
_refine_ls_wR_factor_ref          0.2803
_refine_ls_wR_factor_gt           0.2777
_refine_ls_goodness_of_fit_ref    1.307
_refine_ls_restrained_S_all       1.307
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Pb01 Pb 0.5000 0.0000 0.5000 0.0169(4) Uani 1 2 d S . P . .
Br02 Br 0.52813(5) -0.31225(13) 0.31000(11) 0.0226(4) Uani 1 1 d . . . . .
Br03 Br 0.65965(5) 0.07987(13) 0.49274(11) 0.0232(4) Uani 1 1 d . . . . .
N004 N 0.6415(8) 0.4862(12) 0.5987(17) 0.026(3) Uani 1 1 d . . . . .
H00A H 0.6345 0.3930 0.5387 0.031 Uiso 1 1 calc R U . . .
H00B H 0.6092 0.5662 0.5648 0.031 Uiso 1 1 calc R U . . .
H00C H 0.6353 0.4603 0.6995 0.031 Uiso 1 1 calc R U . . .
C005 C 0.7331(6) 0.5848(13) 0.4197(13) 0.025(2) Uani 1 1 d . . . . .
H00D H 0.7017 0.6768 0.3774 0.030 Uiso 1 1 calc R U . . .
H00E H 0.7212 0.4832 0.3568 0.030 Uiso 1 1 calc R U . . .
C006 C 0.8116(6) 0.6318(14) 0.4048(11) 0.024(2) Uani 1 1 d . . . . .
C007 C 0.7181(6) 0.552(2) 0.5872(14) 0.030(2) Uani 1 1 d . . . . .
H00F H 0.7247 0.6570 0.6479 0.036 Uiso 1 1 calc R U . . .
H00G H 0.7531 0.4687 0.6334 0.036 Uiso 1 1 calc R U . . .
C008 C 0.9070(7) 0.8429(16) 0.4354(14) 0.035(3) Uani 1 1 d . . . . .
H008 H 0.9214 0.9541 0.4620 0.041 Uiso 1 1 calc R U . . .
C009 C 0.9575(6) 0.7355(17) 0.3918(14) 0.035(2) Uani 1 1 d . . . . .
H009 H 1.0056 0.7711 0.3838 0.042 Uiso 1 1 calc R U . . .
C00A C 0.8354(6) 0.8003(14) 0.4437(14) 0.030(2) Uani 1 1 d . . . . .
H00H H 0.8021 0.8813 0.4747 0.036 Uiso 1 1 calc R U . . .
C00B C 0.8634(10) 0.5099(14) 0.354(2) 0.030(4) Uani 1 1 d . . . . .
C00C C 0.8424(8) 0.3315(16) 0.3169(17) 0.040(3) Uani 1 1 d . . . . .
H00I H 0.8151 0.2864 0.4000 0.060 Uiso 1 1 calc R U . . .
H00J H 0.8859 0.2641 0.3087 0.060 Uiso 1 1 calc R U . . .
H00K H 0.8125 0.3277 0.2177 0.060 Uiso 1 1 calc R U . . .
C00D C 0.9364(6) 0.5675(16) 0.3582(14) 0.031(2) Uani 1 1 d . . . . .
H00L H 0.9727 0.4890 0.3373 0.037 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Pb01 Br03 2.9854(9) 3_656 ?
Pb01 Br03 2.9855(9) . ?
Pb01 Br02 2.9882(10) 3_656 ?
Pb01 Br02 2.9882(10) . ?
Pb01 Br02 3.0046(9) 2_655 ?
Pb01 Br02 3.0046(9) 4_556 ?
Br02 Pb01 3.0046(9) 2_645 ?
N004 C007 1.501(18) . ?
N004 H00A 0.8900 . ?
N004 H00B 0.8900 . ?
N004 H00C 0.8900 . ?
C005 C007 1.484(15) . ?
C005 C006 1.494(14) . ?
C005 H00D 0.9700 . ?
C005 H00E 0.9700 . ?
C006 C00B 1.43(2) . ?
C006 C00A 1.417(15) . ?
C007 H00F 0.9700 . ?
C007 H00G 0.9700 . ?
C008 C00A 1.356(17) . ?
C008 C009 1.322(19) . ?
C008 H008 0.9300 . ?
C009 C00D 1.391(18) . ?
C009 H009 0.9300 . ?
C00A H00H 0.9300 . ?
C00B C00D 1.40(2) . ?
C00B C00C 1.473(17) . ?
C00C H00I 0.9600 . ?
C00C H00J 0.9600 . ?
C00C H00K 0.9600 . ?
C00D H00L 0.9300 . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
Br03 Pb01 Br03 180.0 3_656 . ?
Br03 Pb01 Br02 87.02(3) 3_656 3_656 ?
Br03 Pb01 Br02 92.98(3) . 3_656 ?
Br03 Pb01 Br02 92.98(3) 3_656 . ?
Br03 Pb01 Br02 87.02(3) . . ?
Br02 Pb01 Br02 180.0 3_656 . ?
Br03 Pb01 Br02 91.39(3) 3_656 2_655 ?
Br03 Pb01 Br02 88.60(3) . 2_655 ?
Br02 Pb01 Br02 92.461(10) 3_656 2_655 ?
Br02 Pb01 Br02 87.539(11) . 2_655 ?
Br03 Pb01 Br02 88.61(3) 3_656 4_556 ?
Br03 Pb01 Br02 91.40(3) . 4_556 ?
Br02 Pb01 Br02 87.539(10) 3_656 4_556 ?
Br02 Pb01 Br02 92.461(11) . 4_556 ?
Br02 Pb01 Br02 180.0 2_655 4_556 ?
Pb01 Br02 Pb01 147.27(4) . 2_645 ?
C007 N004 H00A 109.5 . . ?
C007 N004 H00B 109.5 . . ?
H00A N004 H00B 109.5 . . ?
C007 N004 H00C 109.5 . . ?
H00A N004 H00C 109.5 . . ?
H00B N004 H00C 109.5 . . ?
C007 C005 C006 112.2(9) . . ?
C007 C005 H00D 109.2 . . ?
C006 C005 H00D 109.2 . . ?
C007 C005 H00E 109.2 . . ?
C006 C005 H00E 109.2 . . ?
H00D C005 H00E 107.9 . . ?
C00B C006 C00A 119.4(11) . . ?
C00B C006 C005 121.5(11) . . ?
C00A C006 C005 119.1(9) . . ?
C005 C007 N004 111.6(10) . . ?
C005 C007 H00F 109.3 . . ?
N004 C007 H00F 109.3 . . ?
C005 C007 H00G 109.3 . . ?
N004 C007 H00G 109.3 . . ?
H00F C007 H00G 108.0 . . ?
C00A C008 C009 123.8(12) . . ?
C00A C008 H008 118.1 . . ?
C009 C008 H008 118.1 . . ?
C008 C009 C00D 118.0(11) . . ?
C008 C009 H009 121.0 . . ?
C00D C009 H009 121.0 . . ?
C008 C00A C006 119.6(11) . . ?
C008 C00A H00H 120.2 . . ?
C006 C00A H00H 120.2 . . ?
C00D C00B C006 115.3(11) . . ?
C00D C00B C00C 122.5(14) . . ?
C006 C00B C00C 121.8(14) . . ?
C00B C00C H00I 109.5 . . ?
C00B C00C H00J 109.5 . . ?
H00I C00C H00J 109.5 . . ?
C00B C00C H00K 109.5 . . ?
H00I C00C H00K 109.5 . . ?
H00J C00C H00K 109.5 . . ?
C009 C00D C00B 123.6(11) . . ?
C009 C00D H00L 118.2 . . ?
C00B C00D H00L 118.2 . . ?
 
_refine_diff_density_max    8.735
_refine_diff_density_min   -4.483
_refine_diff_density_rms    0.646



