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#$Date: 2022-07-01 11:00:26 +0300 (Fri, 01 Jul 2022) $
#$Revision: 276479 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/56/8105608.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_8105608
loop_
_publ_author_name
'Fazal, Atif'
'Fettouhi, Mohammed'
_publ_section_title
;
 Crystal structure of (2,2′-bipyridine-κ 2
 N,N′)bis(4-(dimethylamino)phenyldiphenylphosphane-\kP)copper(I)
 tetrafluoroborate, C50H48BCuF4N4P2
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              253
_journal_page_last               254
_journal_paper_doi               10.1515/ncrs-2018-0289
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C50 H48 Cu N4 P2, B F4'
_chemical_formula_sum            'C50 H48 B Cu F4 N4 P2'
_chemical_formula_weight         917.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.166(2)
_cell_length_b                   19.5652(18)
_cell_length_c                   9.6477(9)
_cell_measurement_reflns_used    7456
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.334
_cell_measurement_theta_min      2.273
_cell_volume                     4561.6(7)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex area detector'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            45154
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.294
_diffrn_reflns_theta_min         1.685
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       plate
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.540
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.029
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         5832
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0907P)²+1.8460P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1546
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4398
_reflns_number_total             5832
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2018-0289_suppl.cif
_cod_data_source_block           shelxl
_cod_database_code               8105608
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.736
_shelx_estimated_absorpt_t_max   0.909
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_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
Cu1 Cu 0.40157(2) 0.2500 0.26915(4) 0.03952(14) Uani 1 2 d S T P . .
N1 N 0.32491(12) 0.2500 0.3719(3) 0.0519(7) Uani 1 2 d S T P . .
N2 N 0.42698(13) 0.2500 0.4782(3) 0.0479(7) Uani 1 2 d S T P . .
N3 N 0.25946(13) 0.02825(15) -0.2266(3) 0.0747(8) Uani 1 1 d . . . . .
P1 P 0.42314(2) 0.14640(3) 0.17719(6) 0.04038(16) Uani 1 1 d . . . . .
C1 C 0.27461(16) 0.2500 0.3161(5) 0.0634(10) Uani 1 2 d S T P . .
H1 H 0.2717 0.2500 0.2200 0.076 Uiso 1 2 calc R U P . .
C2 C 0.22640(17) 0.2500 0.3937(5) 0.0722(12) Uani 1 2 d S T P . .
H2 H 0.1920 0.2500 0.3507 0.087 Uiso 1 2 calc R U P . .
C3 C 0.23060(19) 0.2500 0.5343(6) 0.0758(13) Uani 1 2 d S T P . .
H3 H 0.1989 0.2500 0.5890 0.091 Uiso 1 2 calc R U P . .
C4 C 0.28144(19) 0.2500 0.5943(5) 0.0681(11) Uani 1 2 d S T P . .
H4 H 0.2847 0.2500 0.6903 0.082 Uiso 1 2 calc R U P . .
C5 C 0.32844(16) 0.2500 0.5123(4) 0.0508(8) Uani 1 2 d S T P . .
C6 C 0.38523(17) 0.2500 0.5694(4) 0.0522(8) Uani 1 2 d S T P . .
C7 C 0.3957(2) 0.2500 0.7123(4) 0.0719(13) Uani 1 2 d S T P . .
H7 H 0.3663 0.2500 0.7747 0.086 Uiso 1 2 calc R U P . .
C8 C 0.4487(3) 0.2500 0.7601(5) 0.0829(15) Uani 1 2 d S T P . .
H8 H 0.4558 0.2500 0.8548 0.099 Uiso 1 2 calc R U P . .
C9 C 0.4917(2) 0.2500 0.6664(5) 0.0753(13) Uani 1 2 d S T P . .
H9 H 0.5283 0.2500 0.6962 0.090 Uiso 1 2 calc R U P . .
C10 C 0.47881(17) 0.2500 0.5262(4) 0.0592(9) Uani 1 2 d S T P . .
H10 H 0.5077 0.2500 0.4625 0.071 Uiso 1 2 calc R U P . .
C11 C 0.37850(10) 0.11208(11) 0.0433(2) 0.0424(5) Uani 1 1 d . . . . .
C12 C 0.33199(10) 0.14860(12) 0.0017(3) 0.0468(5) Uani 1 1 d . . . . .
H12 H 0.3269 0.1925 0.0362 0.056 Uiso 1 1 calc R U . . .
C13 C 0.29335(11) 0.12261(13) -0.0881(3) 0.0520(6) Uani 1 1 d . . . . .
H13 H 0.2632 0.1493 -0.1140 0.062 Uiso 1 1 calc R U . . .
C14 C 0.29873(11) 0.05655(14) -0.1410(2) 0.0520(6) Uani 1 1 d . . . . .
C15 C 0.34625(12) 0.01979(14) -0.1030(3) 0.0585(7) Uani 1 1 d . . . . .
H15 H 0.3520 -0.0236 -0.1398 0.070 Uiso 1 1 calc R U . . .
C16 C 0.38461(12) 0.04667(13) -0.0122(3) 0.0529(6) Uani 1 1 d . . . . .
H16 H 0.4152 0.0206 0.0126 0.064 Uiso 1 1 calc R U . . .
C17 C 0.21112(18) 0.0668(2) -0.2656(5) 0.0991(14) Uani 1 1 d . . . . .
H17A H 0.1902 0.0781 -0.1842 0.149 Uiso 1 1 calc R U . . .
H17B H 0.1887 0.0399 -0.3270 0.149 Uiso 1 1 calc R U . . .
H17C H 0.2223 0.1080 -0.3117 0.149 Uiso 1 1 calc R U . . .
C18 C 0.26051(19) -0.0439(2) -0.2592(4) 0.0896(12) Uani 1 1 d . . . . .
H18A H 0.2919 -0.0536 -0.3170 0.134 Uiso 1 1 calc R U . . .
H18B H 0.2272 -0.0561 -0.3073 0.134 Uiso 1 1 calc R U . . .
H18C H 0.2632 -0.0698 -0.1751 0.134 Uiso 1 1 calc R U . . .
C19 C 0.49358(10) 0.14208(11) 0.1106(3) 0.0466(5) Uani 1 1 d . . . . .
C20 C 0.50692(12) 0.13149(15) -0.0266(3) 0.0608(7) Uani 1 1 d . . . . .
H20 H 0.4791 0.1223 -0.0904 0.073 Uiso 1 1 calc R U . . .
C21 C 0.56167(14) 0.13448(17) -0.0704(4) 0.0760(9) Uani 1 1 d . . . . .
H21 H 0.5704 0.1279 -0.1633 0.091 Uiso 1 1 calc R U . . .
C22 C 0.60277(13) 0.14725(17) 0.0240(5) 0.0773(10) Uani 1 1 d . . . . .
H22 H 0.6394 0.1493 -0.0055 0.093 Uiso 1 1 calc R U . . .
C23 C 0.59065(13) 0.15701(17) 0.1609(4) 0.0724(9) Uani 1 1 d . . . . .
H23 H 0.6189 0.1652 0.2242 0.087 Uiso 1 1 calc R U . . .
C24 C 0.53650(12) 0.15470(14) 0.2048(3) 0.0600(7) Uani 1 1 d . . . . .
H24 H 0.5283 0.1616 0.2979 0.072 Uiso 1 1 calc R U . . .
C25 C 0.42184(12) 0.07785(13) 0.3068(3) 0.0520(6) Uani 1 1 d . . . . .
C26 C 0.45628(15) 0.02112(15) 0.3015(3) 0.0687(8) Uani 1 1 d . . . . .
H26 H 0.4837 0.0180 0.2343 0.082 Uiso 1 1 calc R U . . .
C27 C 0.44915(19) -0.03175(18) 0.3994(4) 0.0910(12) Uani 1 1 d . . . . .
H27 H 0.4718 -0.0701 0.3962 0.109 Uiso 1 1 calc R U . . .
C28 C 0.4093(2) -0.0268(2) 0.4984(5) 0.1041(15) Uani 1 1 d . . . . .
H28 H 0.4047 -0.0621 0.5619 0.125 Uiso 1 1 calc R U . . .
C29 C 0.3764(2) 0.0288(2) 0.5054(4) 0.1064(14) Uani 1 1 d . . . . .
H29 H 0.3499 0.0322 0.5750 0.128 Uiso 1 1 calc R U . . .
C30 C 0.38211(16) 0.08114(18) 0.4085(3) 0.0752(9) Uani 1 1 d . . . . .
H30 H 0.3587 0.1188 0.4128 0.090 Uiso 1 1 calc R U . . .
B1 B 0.1546(3) 0.2500 0.9675(7) 0.0918(19) Uani 1 2 d DS T P . .
F1 F 0.1796(3) 0.2500 0.8544(5) 0.237(4) Uani 1 2 d DS T P . .
F2 F 0.1900(3) 0.2500 1.0590(7) 0.359(8) Uani 1 2 d DS T P . .
F3 F 0.1238(3) 0.2992(3) 0.9858(7) 0.283(3) Uani 1 1 d D . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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 Cu1 N2 78.78(12) . .
N1 Cu1 P1 112.73(3) . 7_565
N2 Cu1 P1 107.85(3) . 7_565
N1 Cu1 P1 112.73(3) . .
N2 Cu1 P1 107.85(3) . .
P1 Cu1 P1 126.17(3) 7_565 .
C1 N1 C5 117.5(3) . .
C1 N1 Cu1 127.9(3) . .
C5 N1 Cu1 114.6(2) . .
C10 N2 C6 118.6(3) . .
C10 N2 Cu1 127.2(3) . .
C6 N2 Cu1 114.2(2) . .
C14 N3 C17 120.4(3) . .
C14 N3 C18 120.8(3) . .
C17 N3 C18 117.9(3) . .
C11 P1 C19 106.72(11) . .
C11 P1 C25 101.81(11) . .
C19 P1 C25 102.86(12) . .
C11 P1 Cu1 118.17(8) . .
C19 P1 Cu1 113.17(8) . .
C25 P1 Cu1 112.47(9) . .
N1 C1 C2 123.4(4) . .
N1 C1 H1 118.3 . .
C2 C1 H1 118.3 . .
C3 C2 C1 118.5(4) . .
C3 C2 H2 120.8 . .
C1 C2 H2 120.8 . .
C4 C3 C2 119.5(4) . .
C4 C3 H3 120.3 . .
C2 C3 H3 120.3 . .
C3 C4 C5 119.9(4) . .
C3 C4 H4 120.0 . .
C5 C4 H4 120.0 . .
N1 C5 C4 121.2(4) . .
N1 C5 C6 115.5(3) . .
C4 C5 C6 123.3(4) . .
N2 C6 C7 120.7(4) . .
N2 C6 C5 117.0(3) . .
C7 C6 C5 122.2(4) . .
C8 C7 C6 120.1(4) . .
C8 C7 H7 119.9 . .
C6 C7 H7 119.9 . .
C7 C8 C9 119.2(4) . .
C7 C8 H8 120.4 . .
C9 C8 H8 120.4 . .
C8 C9 C10 118.0(5) . .
C8 C9 H9 121.0 . .
C10 C9 H9 121.0 . .
N2 C10 C9 123.3(4) . .
N2 C10 H10 118.4 . .
C9 C10 H10 118.4 . .
C12 C11 C16 116.5(2) . .
C12 C11 P1 119.78(18) . .
C16 C11 P1 123.40(19) . .
C13 C12 C11 122.8(2) . .
C13 C12 H12 118.6 . .
C11 C12 H12 118.6 . .
C12 C13 C14 120.7(2) . .
C12 C13 H13 119.6 . .
C14 C13 H13 119.6 . .
N3 C14 C13 121.9(3) . .
N3 C14 C15 121.0(3) . .
C13 C14 C15 117.1(2) . .
C16 C15 C14 121.3(2) . .
C16 C15 H15 119.3 . .
C14 C15 H15 119.3 . .
C15 C16 C11 121.5(2) . .
C15 C16 H16 119.3 . .
C11 C16 H16 119.3 . .
N3 C17 H17A 109.5 . .
N3 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
N3 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
N3 C18 H18A 109.5 . .
N3 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
N3 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C20 C19 C24 118.5(3) . .
C20 C19 P1 124.4(2) . .
C24 C19 P1 117.0(2) . .
C19 C20 C21 120.6(3) . .
C19 C20 H20 119.7 . .
C21 C20 H20 119.7 . .
C22 C21 C20 119.7(3) . .
C22 C21 H21 120.1 . .
C20 C21 H21 120.1 . .
C23 C22 C21 120.8(3) . .
C23 C22 H22 119.6 . .
C21 C22 H22 119.6 . .
C22 C23 C24 119.8(3) . .
C22 C23 H23 120.1 . .
C24 C23 H23 120.1 . .
C23 C24 C19 120.7(3) . .
C23 C24 H24 119.7 . .
C19 C24 H24 119.7 . .
C30 C25 C26 118.8(3) . .
C30 C25 P1 117.7(2) . .
C26 C25 P1 123.3(2) . .
C25 C26 C27 119.2(4) . .
C25 C26 H26 120.4 . .
C27 C26 H26 120.4 . .
C28 C27 C26 120.3(4) . .
C28 C27 H27 119.9 . .
C26 C27 H27 119.9 . .
C29 C28 C27 120.7(4) . .
C29 C28 H28 119.7 . .
C27 C28 H28 119.7 . .
C28 C29 C30 120.0(4) . .
C28 C29 H29 120.0 . .
C30 C29 H29 120.0 . .
C25 C30 C29 120.9(4) . .
C25 C30 H30 119.5 . .
C29 C30 H30 119.5 . .
F2 B1 F3 108.6(5) . 7_565
F2 B1 F3 108.6(5) . .
F3 B1 F3 102.9(8) 7_565 .
F2 B1 F1 107.0(7) . .
F3 B1 F1 114.7(5) 7_565 .
F3 B1 F1 114.7(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 2.101(3) .
Cu1 N2 2.108(3) .
Cu1 P1 2.2732(6) 7_565
Cu1 P1 2.2732(6) .
N1 C1 1.329(5) .
N1 C5 1.357(5) .
N2 C10 1.335(5) .
N2 C6 1.339(5) .
N3 C14 1.375(3) .
N3 C17 1.440(5) .
N3 C18 1.446(5) .
P1 C11 1.812(2) .
P1 C19 1.821(2) .
P1 C25 1.834(3) .
C1 C2 1.385(6) .
C1 H1 0.9300 .
C2 C3 1.360(7) .
C2 H2 0.9300 .
C3 C4 1.358(7) .
C3 H3 0.9300 .
C4 C5 1.384(5) .
C4 H4 0.9300 .
C5 C6 1.479(5) .
C6 C7 1.402(5) .
C7 C8 1.362(7) .
C7 H7 0.9300 .
C8 C9 1.377(8) .
C8 H8 0.9300 .
C9 C10 1.388(6) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 C12 1.391(3) .
C11 C16 1.395(3) .
C12 C13 1.371(3) .
C12 H12 0.9300 .
C13 C14 1.396(4) .
C13 H13 0.9300 .
C14 C15 1.404(4) .
C15 C16 1.380(4) .
C15 H15 0.9300 .
C16 H16 0.9300 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C19 C20 1.378(4) .
C19 C24 1.401(4) .
C20 C21 1.390(4) .
C20 H20 0.9300 .
C21 C22 1.370(5) .
C21 H21 0.9300 .
C22 C23 1.366(6) .
C22 H22 0.9300 .
C23 C24 1.376(4) .
C23 H23 0.9300 .
C24 H24 0.9300 .
C25 C30 1.375(4) .
C25 C26 1.388(4) .
C26 C27 1.411(5) .
C26 H26 0.9300 .
C27 C28 1.359(6) .
C27 H27 0.9300 .
C28 C29 1.350(7) .
C28 H28 0.9300 .
C29 C30 1.394(5) .
C29 H29 0.9300 .
C30 H30 0.9300 .
B1 F2 1.228(8) .
B1 F3 1.230(5) 7_565
B1 F3 1.230(5) .
B1 F1 1.247(7) .
