#------------------------------------------------------------------------------
#$Date: 2019-11-23 20:58:16 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234964 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/34/1553410.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1553410
loop_
_publ_author_name
'Sui, Xuelin'
'Hong, Changwen'
'Pang, Wenmin'
'Chen, Changle'
_publ_section_title
;
 Unsymmetrical α-diimine palladium catalysts and their properties in
 olefin (co)polymerization
;
_journal_issue                   5
_journal_name_full               'Materials Chemistry Frontiers'
_journal_page_first              967
_journal_paper_doi               10.1039/C6QM00235H
_journal_volume                  1
_journal_year                    2017
_chemical_formula_sum            'C46 H44 Br2 N2 Ni'
_chemical_formula_weight         843.36
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-09-24 deposited with the CCDC.
2016-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.927(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6692(2)
_cell_length_b                   15.1682(3)
_cell_length_c                   28.4042(5)
_cell_measurement_reflns_used    3447
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.60
_cell_measurement_theta_min      2.56
_cell_volume                     4143.61(14)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0190
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7632
_diffrn_reflns_theta_full        71.28
_diffrn_reflns_theta_max         71.28
_diffrn_reflns_theta_min         5.45
_exptl_absorpt_coefficient_mu    3.173
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.263
_refine_diff_density_min         -2.248
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         3880
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.1202
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1702P)²+30.6662P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3249
_refine_ls_wR_factor_ref         0.3336
_reflns_number_gt                3447
_reflns_number_total             3880
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qm00235h2.cif
_cod_data_source_block           111
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               1553410
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.5000 0.12172(10) 0.7500 0.0733(6) Uani 1 2 d S
Br1 Br 0.3040(3) 0.05136(14) 0.76987(5) 0.2335(16) Uani 1 1 d .
C2 C 0.4066(5) 0.1914(4) 0.62314(18) 0.0438(11) Uani 1 1 d .
N1 N 0.4308(4) 0.2210(3) 0.70837(15) 0.0434(10) Uani 1 1 d .
C9 C 0.5643(5) 0.1896(4) 0.62423(18) 0.0443(12) Uani 1 1 d .
H9 H 0.5994 0.1620 0.6543 0.053 Uiso 1 1 calc R
C21 C 0.5586(8) 0.3499(5) 0.5990(2) 0.0635(16) Uani 1 1 d .
H21 H 0.4776 0.3388 0.5792 0.076 Uiso 1 1 calc R
C11 C 0.6520(8) 0.1649(6) 0.5433(2) 0.0715(19) Uani 1 1 d .
H11 H 0.6528 0.2257 0.5390 0.086 Uiso 1 1 calc R
C3 C 0.3200(6) 0.1797(4) 0.58131(19) 0.0512(13) Uani 1 1 d .
H3 H 0.3595 0.1663 0.5537 0.061 Uiso 1 1 calc R
C17 C 0.7422(7) 0.3008(5) 0.6541(3) 0.0680(17) Uani 1 1 d .
H17 H 0.7870 0.2562 0.6722 0.082 Uiso 1 1 calc R
C16 C 0.6228(6) 0.2821(4) 0.62537(19) 0.0474(12) Uani 1 1 d .
C5 C 0.1192(7) 0.2072(8) 0.6211(3) 0.090(3) Uani 1 1 d .
H5 H 0.0232 0.2129 0.6202 0.108 Uiso 1 1 calc R
C1 C 0.3449(6) 0.2110(4) 0.66401(19) 0.0514(13) Uani 1 1 d .
C23 C 0.4161(12) 0.3833(5) 0.7040(3) 0.089(3) Uani 1 1 d .
H23A H 0.4962 0.4205 0.7033 0.134 Uiso 1 1 calc R
H23B H 0.3498 0.4114 0.7220 0.134 Uiso 1 1 calc R
H23C H 0.3747 0.3732 0.6723 0.134 Uiso 1 1 calc R
C4 C 0.1776(7) 0.1873(5) 0.5796(2) 0.0660(17) Uani 1 1 d .
C20 C 0.6140(11) 0.4350(5) 0.6017(3) 0.085(2) Uani 1 1 d .
H20 H 0.5697 0.4799 0.5836 0.102 Uiso 1 1 calc R
C10 C 0.6131(6) 0.1316(4) 0.5851(2) 0.0538(14) Uani 1 1 d .
C19 C 0.7312(11) 0.4528(6) 0.6303(4) 0.093(3) Uani 1 1 d .
H19 H 0.7668 0.5098 0.6322 0.111 Uiso 1 1 calc R
C6 C 0.2007(7) 0.2187(7) 0.6637(3) 0.084(3) Uani 1 1 d .
C14 C 0.6579(14) -0.0138(7) 0.5561(5) 0.119(4) Uani 1 1 d .
H14 H 0.6595 -0.0746 0.5606 0.143 Uiso 1 1 calc R
C8 C 0.1316(9) 0.2413(13) 0.7084(4) 0.147(6) Uani 1 1 d .
H8A H 0.2004 0.2636 0.7322 0.221 Uiso 1 1 calc R
H8B H 0.0899 0.1892 0.7199 0.221 Uiso 1 1 calc R
H8C H 0.0613 0.2853 0.7010 0.221 Uiso 1 1 calc R
C15 C 0.6188(10) 0.0417(6) 0.5916(3) 0.088(2) Uani 1 1 d .
H15 H 0.5962 0.0176 0.6199 0.106 Uiso 1 1 calc R
C7 C 0.0854(9) 0.1771(8) 0.5336(3) 0.095(3) Uani 1 1 d .
H7A H 0.0106 0.1375 0.5381 0.143 Uiso 1 1 calc R
H7B H 0.1390 0.1538 0.5098 0.143 Uiso 1 1 calc R
H7C H 0.0482 0.2335 0.5236 0.143 Uiso 1 1 calc R
C12 C 0.6901(9) 0.1110(7) 0.5075(3) 0.094(3) Uani 1 1 d .
H12 H 0.7125 0.1349 0.4791 0.113 Uiso 1 1 calc R
C18 C 0.7975(10) 0.3863(7) 0.6567(4) 0.100(3) Uani 1 1 d .
H18 H 0.8788 0.3980 0.6761 0.120 Uiso 1 1 calc R
C13 C 0.6939(11) 0.0212(8) 0.5148(4) 0.113(4) Uani 1 1 d .
H13 H 0.7213 -0.0158 0.4914 0.135 Uiso 1 1 calc R
C22 C 0.4592(6) 0.2971(4) 0.72648(19) 0.0483(13) Uani 1 1 d .
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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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'
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
N1 Ni1 N1 81.5(3) 2_656 .
N1 Ni1 Br1 116.22(13) 2_656 .
N1 Ni1 Br1 105.24(14) . .
N1 Ni1 Br1 105.24(14) 2_656 2_656
N1 Ni1 Br1 116.22(13) . 2_656
Br1 Ni1 Br1 124.59(16) . 2_656
C3 C2 C1 117.8(5) . .
C3 C2 C9 121.9(5) . .
C1 C2 C9 120.1(5) . .
C22 N1 C1 121.7(5) . .
C22 N1 Ni1 113.5(4) . .
C1 N1 Ni1 124.6(4) . .
C16 C9 C10 114.0(5) . .
C16 C9 C2 110.8(5) . .
C10 C9 C2 112.3(4) . .
C16 C21 C20 120.6(7) . .
C10 C11 C12 122.3(8) . .
C2 C3 C4 122.0(5) . .
C16 C17 C18 120.9(8) . .
C21 C16 C17 118.2(6) . .
C21 C16 C9 122.2(5) . .
C17 C16 C9 119.6(6) . .
C6 C5 C4 121.5(6) . .
C2 C1 C6 121.8(5) . .
C2 C1 N1 119.5(5) . .
C6 C1 N1 118.7(5) . .
C3 C4 C5 118.7(6) . .
C3 C4 C7 121.3(7) . .
C5 C4 C7 120.0(7) . .
C19 C20 C21 120.7(9) . .
C15 C10 C11 117.8(7) . .
C15 C10 C9 119.0(6) . .
C11 C10 C9 123.2(6) . .
C20 C19 C18 119.7(8) . .
C5 C6 C1 118.1(6) . .
C5 C6 C8 119.6(7) . .
C1 C6 C8 122.2(7) . .
C13 C14 C15 119.9(10) . .
C10 C15 C14 120.8(10) . .
C11 C12 C13 118.6(9) . .
C19 C18 C17 119.8(8) . .
C14 C13 C12 120.6(8) . .
N1 C22 C22 115.8(3) . 2_656
N1 C22 C23 125.2(6) . .
C22 C22 C23 119.0(4) 2_656 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 1.988(5) 2_656
Ni1 N1 1.988(5) .
Ni1 Br1 2.2956(18) .
Ni1 Br1 2.2956(18) 2_656
C2 C3 1.393(7) .
C2 C1 1.391(8) .
C2 C9 1.522(7) .
N1 C22 1.281(7) .
N1 C1 1.444(7) .
C9 C16 1.513(8) .
C9 C10 1.529(7) .
C21 C16 1.381(9) .
C21 C20 1.396(11) .
C11 C10 1.378(10) .
C11 C12 1.385(10) .
C3 C4 1.377(9) .
C17 C16 1.373(9) .
C17 C18 1.401(12) .
C5 C6 1.387(10) .
C5 C4 1.391(11) .
C1 C6 1.398(9) .
C23 C22 1.495(8) .
C4 C7 1.512(9) .
C20 C19 1.352(14) .
C10 C15 1.377(11) .
C19 C18 1.375(14) .
C6 C8 1.533(11) .
C14 C13 1.366(17) .
C14 C15 1.395(13) .
C12 C13 1.378(16) .
C22 C22 1.480(11) 2_656
