####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_pdcycp180_0m_a
_audit_block_doi                 10.5517/ccdc.csd.cc1kndl6
_database_code_depnum_ccdc_archive 'CCDC 1449578'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1002/slct.201600065 2016
_audit_update_record             
;
2016-01-25 deposited with the CCDC.	2022-04-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[Pd(cptn)2Br]Br2'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H24 Br3 N4 Pd'
_chemical_formula_weight         546.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           23
_space_group_name_H-M_alt        'I 2 2 2'
_space_group_name_Hall           'I 2 2'

_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, z'
'x, -y, -z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'

_cell_length_a                   5.2223(4)
_cell_length_b                   6.9660(5)
_cell_length_c                   22.6349(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     823.42(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    193
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.204
_exptl_crystal_F_000             526
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    8.396
_shelx_estimated_absorpt_T_min   0.260
_shelx_estimated_absorpt_T_max   0.553
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.2584
_exptl_absorpt_correction_T_max  0.5390
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'APEXII CCD diffractometer'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2450
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.799
_diffrn_reflns_theta_max         26.321
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             856
_reflns_number_gt                812
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.634
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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)+(0.0111P)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_abs_structure_details 
;
 Flack x determined using 291 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(3)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         856
_refine_ls_number_parameters     44
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0174
_refine_ls_wR_factor_ref         0.0388
_refine_ls_wR_factor_gt          0.0384
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.049
_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
Pd1 Pd 0.5000 1.0000 1.0000 0.00519(13) Uani 1 4 d S TU P . .
Br1 Br 0.0000 1.0000 1.0000 0.01087(16) Uani 1 4 d S TU P . .
Br2 Br 0.0000 0.5000 0.90425(2) 0.01345(13) Uani 1 2 d S T P . .
N1 N 0.495(2) 0.7982(3) 0.93287(12) 0.0091(6) Uani 1 1 d . U . . .
H1A H 0.6507 0.7412 0.9291 0.011 Uiso 1 1 calc R U . . .
H1B H 0.3756 0.7060 0.9403 0.011 Uiso 1 1 calc R U . . .
C1 C 0.4285(7) 0.9060(5) 0.87845(18) 0.0112(10) Uani 1 1 d . U . . .
H1 H 0.2411 0.9350 0.8796 0.013 Uiso 1 1 calc R U . . .
C2 C 0.490(3) 0.8203(5) 0.81820(15) 0.0179(10) Uani 1 1 d . U . . .
H2A H 0.3545 0.7304 0.8052 0.021 Uiso 1 1 calc R U . . .
H2B H 0.6566 0.7525 0.8186 0.021 Uiso 1 1 calc R U . . .
C3 C 0.5000 1.0000 0.7783(3) 0.058(3) Uani 1 2 d S TU P . .
H3A H 0.3464 1.0048 0.7527 0.069 Uiso 0.5 1 calc R U P . .
H3B H 0.6536 0.9952 0.7527 0.069 Uiso 0.5 1 calc R U P . .


_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
Pd1 N1 2.070(3) 3_577 ?
Pd1 N1 2.070(3) 2_675 ?
Pd1 N1 2.070(3) 4_657 ?
Pd1 N1 2.070(3) . ?
Pd1 Br1 2.6111(2) 1_655 ?
Pd1 Br1 2.6111(2) . ?
Br1 Pd1 2.6111(2) 1_455 ?
N1 C1 1.483(5) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
C1 C1 1.508(7) 2_675 ?
C1 C2 1.523(6) . ?
C1 H1 1.0000 . ?
C2 C3 1.545(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C2 1.545(5) 2_675 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?

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
N1 Pd1 N1 94.45(14) 3_577 2_675 ?
N1 Pd1 N1 85.57(14) 3_577 4_657 ?
N1 Pd1 N1 178.5(6) 2_675 4_657 ?
N1 Pd1 N1 178.5(6) 3_577 . ?
N1 Pd1 N1 85.57(14) 2_675 . ?
N1 Pd1 N1 94.45(14) 4_657 . ?
N1 Pd1 Br1 90.8(3) 3_577 1_655 ?
N1 Pd1 Br1 89.2(3) 2_675 1_655 ?
N1 Pd1 Br1 89.2(3) 4_657 1_655 ?
N1 Pd1 Br1 90.8(3) . 1_655 ?
N1 Pd1 Br1 89.2(3) 3_577 . ?
N1 Pd1 Br1 90.8(3) 2_675 . ?
N1 Pd1 Br1 90.8(3) 4_657 . ?
N1 Pd1 Br1 89.2(3) . . ?
Br1 Pd1 Br1 180.0 1_655 . ?
Pd1 Br1 Pd1 180.0 1_455 . ?
C1 N1 Pd1 105.6(2) . . ?
C1 N1 H1A 110.6 . . ?
Pd1 N1 H1A 110.6 . . ?
C1 N1 H1B 110.6 . . ?
Pd1 N1 H1B 110.6 . . ?
H1A N1 H1B 108.8 . . ?
N1 C1 C1 108.9(3) . 2_675 ?
N1 C1 C2 119.8(4) . . ?
C1 C1 C2 103.6(4) 2_675 . ?
N1 C1 H1 108.0 . . ?
C1 C1 H1 108.0 2_675 . ?
C2 C1 H1 108.0 . . ?
C1 C2 C3 102.4(3) . . ?
C1 C2 H2A 111.3 . . ?
C3 C2 H2A 111.3 . . ?
C1 C2 H2B 111.3 . . ?
C3 C2 H2B 111.3 . . ?
H2A C2 H2B 109.2 . . ?
C2 C3 C2 108.4(5) . 2_675 ?
C2 C3 H3A 110.0 . . ?
C2 C3 H3A 110.0 2_675 . ?
C2 C3 H3B 110.0 . . ?
C2 C3 H3B 110.0 2_675 . ?
H3A C3 H3B 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 N1 C1 C1 41.3(6) . . . 2_675 ?
Pd1 N1 C1 C2 160.3(8) . . . . ?
N1 C1 C2 C3 -157.2(7) . . . . ?
C1 C1 C2 C3 -35.7(10) 2_675 . . . ?
C1 C2 C3 C2 13.4(3) . . . 2_675 ?

_refine_diff_density_max         0.629
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.095



