#------------------------------------------------------------------------------
#$Date: 2022-10-13 01:14:15 +0300 (Thu, 13 Oct 2022) $
#$Revision: 278552 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/77/1567767.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_1567767
loop_
_publ_author_name
'Sharma, Mahendra K.'
'Chabbra, Sonia'
'Wölper, Christoph'
'Weinert, Hanns Micha'
'Reijerse, Edward'
'Schnegg, Alexander'
'Schulz, Stephan'
_publ_section_title
;
 Modulating the Frontier Orbitals of L(X)Ga-Substituted Diphosphenes
 [L(X)GaP]2 (X = Cl, Br) and their Facile Oxidation to Radical Cations
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC04207J
_journal_year                    2022
_chemical_formula_sum            'C58 H82 Cl2 Ga2 N4 P2'
_chemical_formula_weight         1107.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-07-05 deposited with the CCDC.	2022-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.336(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.7010(18)
_cell_length_b                   13.8715(16)
_cell_length_c                   15.7041(18)
_cell_measurement_reflns_used    9679
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.14
_cell_measurement_theta_min      2.69
_cell_volume                     2878.3(6)
_computing_cell_refinement       'BRUKER APEX3(v2019.1-0)'
_computing_data_collection       'BRUKER APEX3(v2019.1-0)'
_computing_data_reduction        'BRUKER APEX3(v2019.1-0)'
_computing_molecular_graphics    'ORTEP/PLATON (Spek)'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'BRUKER APEX3(v2019.1-0)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 KAPPA II (APEX II detector)'
_diffrn_measurement_method       'Data collection strategy APEX 2/COSMO'
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            72672
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         40.215
_diffrn_reflns_theta_min         1.991
_exptl_absorpt_coefficient_mu    1.124
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            'greenish yellow'
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.452
_exptl_crystal_size_mid          0.402
_exptl_crystal_size_min          0.368
_refine_diff_density_max         1.096
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         18029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0459P)²+0.6679P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14347
_reflns_number_total             18029
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2sc04207j2.cif
_cod_data_source_block           mks_001m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1567767
_shelx_shelxl_version_number     2017/1
_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   0.631
_shelx_estimated_absorpt_t_max   0.683
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Ga1 Ga 0.05089(2) 0.13275(2) 0.62152(2) 0.01090(2) Uani 1 1 d . . . . .
Cl1 Cl 0.17261(2) 0.06680(2) 0.72780(2) 0.02082(4) Uani 1 1 d . . . . .
P1 P -0.05565(2) 0.02967(2) 0.52365(2) 0.02004(5) Uani 1 1 d . . . . .
N1 N 0.12000(5) 0.23320(5) 0.57372(4) 0.01175(10) Uani 1 1 d . . . . .
N2 N -0.02279(5) 0.21625(5) 0.68146(4) 0.01227(10) Uani 1 1 d . . . . .
C1 C 0.14150(6) 0.31567(6) 0.61850(5) 0.01433(12) Uani 1 1 d . . . . .
C2 C 0.10070(7) 0.34190(6) 0.68893(6) 0.01688(13) Uani 1 1 d . . . . .
H2 H 0.132720 0.394500 0.724164 0.020 Uiso 1 1 calc R U . . .
C3 C 0.01857(6) 0.30000(6) 0.71358(5) 0.01443(12) Uani 1 1 d . . . . .
C4 C 0.21247(8) 0.38703(7) 0.59364(7) 0.02349(18) Uani 1 1 d . . . . .
H4A H 0.200245 0.388396 0.529276 0.035 Uiso 1 1 calc R U . . .
H4B H 0.282629 0.367704 0.620715 0.035 Uiso 1 1 calc R U . . .
H4C H 0.200621 0.451321 0.614775 0.035 Uiso 1 1 calc R U . . .
C5 C -0.02340(8) 0.35396(7) 0.77978(7) 0.02208(17) Uani 1 1 d . . . . .
H5A H -0.025885 0.423042 0.766317 0.033 Uiso 1 1 calc R U . . .
H5B H 0.020290 0.343141 0.839376 0.033 Uiso 1 1 calc R U . . .
H5C H -0.091813 0.330647 0.776542 0.033 Uiso 1 1 calc R U . . .
C6 C 0.15325(6) 0.21441(6) 0.49516(5) 0.01229(11) Uani 1 1 d . . . . .
C7 C 0.24928(6) 0.17390(6) 0.50184(5) 0.01347(12) Uani 1 1 d . . . . .
C8 C 0.27566(7) 0.15117(7) 0.42385(6) 0.01886(15) Uani 1 1 d . . . . .
H8 H 0.339883 0.123161 0.427397 0.023 Uiso 1 1 calc R U . . .
C9 C 0.21012(8) 0.16868(9) 0.34184(6) 0.02300(17) Uani 1 1 d . . . . .
H9 H 0.229632 0.153755 0.289634 0.028 Uiso 1 1 calc R U . . .
C10 C 0.11577(8) 0.20816(9) 0.33642(6) 0.02438(19) Uani 1 1 d . . . . .
H10 H 0.071171 0.220366 0.279918 0.029 Uiso 1 1 calc R U . . .
C11 C 0.08458(7) 0.23046(8) 0.41180(6) 0.01961(15) Uani 1 1 d . . . . .
C12 C 0.32496(6) 0.15243(7) 0.58951(6) 0.01722(14) Uani 1 1 d . . . . .
H12 H 0.295979 0.175573 0.637986 0.021 Uiso 1 1 calc R U . . .
C13 C 0.42562(8) 0.20489(10) 0.59758(7) 0.0268(2) Uani 1 1 d . . . . .
H13A H 0.455037 0.183329 0.550345 0.040 Uiso 1 1 calc R U . . .
H13B H 0.472455 0.190291 0.655022 0.040 Uiso 1 1 calc R U . . .
H13C H 0.413632 0.274566 0.592523 0.040 Uiso 1 1 calc R U . . .
C14 C 0.34447(9) 0.04391(9) 0.60145(8) 0.0282(2) Uani 1 1 d . . . . .
H14A H 0.279976 0.010089 0.594137 0.042 Uiso 1 1 calc R U . . .
H14B H 0.388274 0.031405 0.660688 0.042 Uiso 1 1 calc R U . . .
H14C H 0.377644 0.020798 0.557157 0.042 Uiso 1 1 calc R U . . .
C15 C -0.0248(4) 0.2620(3) 0.4025(3) 0.0179(6) Uani 0.53(2) 1 d . . P A 1
H15 H -0.043684 0.241658 0.457103 0.021 Uiso 0.53(2) 1 calc R U P A 1
C16 C -0.0299(3) 0.3716(3) 0.3977(6) 0.0417(13) Uani 0.53(2) 1 d . . P A 1
H16A H -0.007643 0.393721 0.346616 0.063 Uiso 0.53(2) 1 calc R U P A 1
H16B H 0.014402 0.398860 0.451804 0.063 Uiso 0.53(2) 1 calc R U P A 1
H16C H -0.099656 0.392651 0.391644 0.063 Uiso 0.53(2) 1 calc R U P A 1
C17 C -0.1017(5) 0.2178(4) 0.3232(4) 0.0219(7) Uani 0.53(2) 1 d . . P A 1
H17A H -0.087696 0.240306 0.268492 0.033 Uiso 0.53(2) 1 calc R U P A 1
H17B H -0.170163 0.237445 0.324054 0.033 Uiso 0.53(2) 1 calc R U P A 1
H17C H -0.096507 0.147378 0.326393 0.033 Uiso 0.53(2) 1 calc R U P A 1
C15' C -0.0142(6) 0.2875(9) 0.4017(5) 0.0334(15) Uani 0.47(2) 1 d . . P A 2
H15' H -0.030757 0.286420 0.459963 0.040 Uiso 0.47(2) 1 calc R U P A 2
C16' C -0.0084(8) 0.3933(7) 0.3751(4) 0.0495(18) Uani 0.47(2) 1 d . . P A 2
H16D H 0.012831 0.396687 0.320340 0.074 Uiso 0.47(2) 1 calc R U P A 2
H16E H 0.040669 0.427524 0.422127 0.074 Uiso 0.47(2) 1 calc R U P A 2
H16F H -0.075202 0.423257 0.365964 0.074 Uiso 0.47(2) 1 calc R U P A 2
C17' C -0.0997(7) 0.2377(10) 0.3349(7) 0.047(2) Uani 0.47(2) 1 d . . P A 2
H17D H -0.082801 0.232987 0.278227 0.071 Uiso 0.47(2) 1 calc R U P A 2
H17E H -0.162133 0.275068 0.327359 0.071 Uiso 0.47(2) 1 calc R U P A 2
H17F H -0.109453 0.172902 0.356131 0.071 Uiso 0.47(2) 1 calc R U P A 2
C18 C -0.11896(6) 0.18318(6) 0.69224(5) 0.01309(11) Uani 1 1 d . . . . .
C19 C -0.12251(7) 0.12164(6) 0.76262(6) 0.01630(13) Uani 1 1 d . . . . .
C20 C -0.21665(8) 0.08497(8) 0.76608(7) 0.02270(17) Uani 1 1 d . . . . .
H20 H -0.220297 0.043232 0.813096 0.027 Uiso 1 1 calc R U . . .
C21 C -0.30452(8) 0.10832(9) 0.70236(8) 0.02628(19) Uani 1 1 d . . . . .
H21 H -0.367620 0.082441 0.705629 0.032 Uiso 1 1 calc R U . . .
C22 C -0.29998(7) 0.16969(9) 0.63373(7) 0.02486(18) Uani 1 1 d . . . . .
H22 H -0.360585 0.186129 0.590620 0.030 Uiso 1 1 calc R U . . .
C23 C -0.20788(7) 0.20778(7) 0.62682(6) 0.01764(14) Uani 1 1 d . . . . .
C24 C -0.02918(7) 0.09401(8) 0.83494(6) 0.02001(15) Uani 1 1 d . . . . .
H24 H 0.030097 0.129228 0.824133 0.024 Uiso 1 1 calc R U . . .
C25 C -0.04075(10) 0.12448(11) 0.92566(7) 0.0323(2) Uani 1 1 d . . . . .
H25A H -0.053634 0.193977 0.925618 0.048 Uiso 1 1 calc R U . . .
H25B H 0.021582 0.109350 0.971114 0.048 Uiso 1 1 calc R U . . .
H25C H -0.097572 0.089592 0.938205 0.048 Uiso 1 1 calc R U . . .
C26 C -0.00791(9) -0.01443(9) 0.83358(8) 0.0288(2) Uani 1 1 d . . . . .
H26A H 0.000531 -0.032495 0.775620 0.043 Uiso 1 1 calc R U . . .
H26B H -0.064774 -0.050365 0.844910 0.043 Uiso 1 1 calc R U . . .
H26C H 0.054099 -0.029729 0.879345 0.043 Uiso 1 1 calc R U . . .
C27 C -0.20637(8) 0.27591(9) 0.55114(7) 0.02567(19) Uani 1 1 d . . . . .
H27 H -0.136128 0.276451 0.543650 0.031 Uiso 1 1 calc R U . . .
C28 C -0.23265(13) 0.37943(10) 0.57320(10) 0.0398(3) Uani 1 1 d . . . . .
H28A H -0.232926 0.421995 0.523328 0.060 Uiso 1 1 calc R U . . .
H28B H -0.182043 0.402108 0.625862 0.060 Uiso 1 1 calc R U . . .
H28C H -0.299692 0.379984 0.584420 0.060 Uiso 1 1 calc R U . . .
C29 C -0.27852(11) 0.24398(11) 0.46347(8) 0.0351(3) Uani 1 1 d . . . . .
H29A H -0.271015 0.287019 0.416124 0.053 Uiso 1 1 calc R U . . .
H29B H -0.348420 0.246692 0.468078 0.053 Uiso 1 1 calc R U . . .
H29C H -0.262269 0.177811 0.450159 0.053 Uiso 1 1 calc R U . . .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'
P P 0.1023 0.0942 '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
_geom_angle_publ_flag
N2 Ga1 N1 97.40(3) . . ?
N2 Ga1 Cl1 105.39(2) . . ?
N1 Ga1 Cl1 103.88(2) . . ?
N2 Ga1 P1 111.98(2) . . ?
N1 Ga1 P1 118.22(2) . . ?
Cl1 Ga1 P1 117.464(13) . . ?
P1 P1 Ga1 95.182(18) 3_556 . ?
C1 N1 C6 121.88(7) . . ?
C1 N1 Ga1 118.25(5) . . ?
C6 N1 Ga1 119.70(5) . . ?
C3 N2 C18 122.80(6) . . ?
C3 N2 Ga1 118.79(5) . . ?
C18 N2 Ga1 118.38(5) . . ?
N1 C1 C2 123.75(7) . . ?
N1 C1 C4 119.57(7) . . ?
C2 C1 C4 116.68(7) . . ?
C3 C2 C1 128.26(7) . . ?
N2 C3 C2 123.14(7) . . ?
N2 C3 C5 119.40(7) . . ?
C2 C3 C5 117.47(7) . . ?
C7 C6 C11 120.77(7) . . ?
C7 C6 N1 120.44(7) . . ?
C11 C6 N1 118.60(7) . . ?
C8 C7 C6 118.44(7) . . ?
C8 C7 C12 118.45(7) . . ?
C6 C7 C12 123.10(7) . . ?
C9 C8 C7 121.36(8) . . ?
C8 C9 C10 119.48(8) . . ?
C9 C10 C11 121.70(9) . . ?
C10 C11 C6 118.21(8) . . ?
C10 C11 C15 119.6(2) . . ?
C6 C11 C15 121.9(2) . . ?
C10 C11 C15' 119.0(3) . . ?
C6 C11 C15' 121.9(3) . . ?
C7 C12 C14 111.04(8) . . ?
C7 C12 C13 111.42(8) . . ?
C14 C12 C13 109.39(9) . . ?
C16 C15 C17 110.3(4) . . ?
C16 C15 C11 108.7(3) . . ?
C17 C15 C11 114.1(4) . . ?
C17' C15' C16' 109.5(6) . . ?
C17' C15' C11 109.5(6) . . ?
C16' C15' C11 114.5(5) . . ?
C19 C18 C23 121.04(8) . . ?
C19 C18 N2 120.39(7) . . ?
C23 C18 N2 118.38(7) . . ?
C20 C19 C18 118.30(8) . . ?
C20 C19 C24 118.78(8) . . ?
C18 C19 C24 122.92(8) . . ?
C21 C20 C19 121.36(9) . . ?
C20 C21 C22 119.71(9) . . ?
C21 C22 C23 121.25(9) . . ?
C22 C23 C18 118.34(8) . . ?
C22 C23 C27 119.59(8) . . ?
C18 C23 C27 122.05(8) . . ?
C19 C24 C26 111.28(9) . . ?
C19 C24 C25 110.60(8) . . ?
C26 C24 C25 110.48(9) . . ?
C23 C27 C29 112.52(10) . . ?
C23 C27 C28 110.52(10) . . ?
C29 C27 C28 109.72(10) . . ?
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
Ga1 N2 1.9363(7) . ?
Ga1 N1 1.9436(7) . ?
Ga1 Cl1 2.2207(3) . ?
Ga1 P1 2.3131(3) . ?
P1 P1 2.0381(5) 3_556 ?
N1 C1 1.3344(10) . ?
N1 C6 1.4473(10) . ?
N2 C3 1.3320(11) . ?
N2 C18 1.4469(10) . ?
C1 C2 1.4127(12) . ?
C1 C4 1.5095(12) . ?
C2 C3 1.4085(12) . ?
C3 C5 1.5127(11) . ?
C6 C7 1.4089(11) . ?
C6 C11 1.4132(12) . ?
C7 C8 1.4015(11) . ?
C7 C12 1.5179(12) . ?
C8 C9 1.3828(13) . ?
C9 C10 1.3856(14) . ?
C10 C11 1.3955(13) . ?
C11 C15 1.531(5) . ?
C11 C15' 1.539(7) . ?
C12 C14 1.5317(15) . ?
C12 C13 1.5347(14) . ?
C15 C16 1.522(5) . ?
C15 C17 1.530(7) . ?
C15' C17' 1.517(11) . ?
C15' C16' 1.533(7) . ?
C18 C19 1.4076(12) . ?
C18 C23 1.4121(12) . ?
C19 C20 1.4007(13) . ?
C19 C24 1.5178(13) . ?
C20 C21 1.3850(16) . ?
C21 C22 1.3876(16) . ?
C22 C23 1.3985(13) . ?
C23 C27 1.5227(14) . ?
C24 C26 1.5334(16) . ?
C24 C25 1.5339(15) . ?
C27 C29 1.5327(18) . ?
C27 C28 1.542(2) . ?
