#------------------------------------------------------------------------------
#$Date: 2020-08-06 15:48:34 +0300 (Thu, 06 Aug 2020) $
#$Revision: 254866 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/66/7126698.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_7126698
loop_
_publ_author_name
'Kroll, Alexander'
'Steinert, Henning'
'Scharf, Lennart T.'
'Scherpf, Thorsten'
'Mallick, Bert'
'Gessner, Viktoria H.'
_publ_section_title
;
 A diamino-substituted carbodiphosphorane as strong C-donor and weak
 N-donor: isolation of monomeric trigonal-planar
 L·ZnCl₂.
;
_journal_issue                   58
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8051
_journal_page_last               8054
_journal_paper_doi               10.1039/d0cc02496a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C35 H40 Cl3 Ga N2 P2'
_chemical_formula_sum            'C35 H40 Cl3 Ga N2 P2'
_chemical_formula_weight         726.70
_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
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2020-03-27 deposited with the CCDC.	2020-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.0445(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.22942(16)
_cell_length_b                   18.8800(3)
_cell_length_c                   17.9216(2)
_cell_measurement_reflns_used    29947
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.2020
_cell_measurement_theta_min      3.3970
_cell_volume                     3357.76(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0056
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11224
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.122
_diffrn_reflns_theta_max         67.122
_diffrn_reflns_theta_min         3.456
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.430
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.20a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.086
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.014
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         11224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0325
_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)+(0.0475P)²+1.9210P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10691
_reflns_number_total             11224
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc02496a2.cif
_cod_data_source_block           AK-032_twin1_hklf5
_cod_depositor_comments
'Adding full bibliography for 7126695--7126700.cif.'
_cod_original_cell_volume        3357.77(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7126698
_shelx_shelxl_version_number     2018/1
_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.
;
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 0.26248(3) 0.31212(2) 0.73608(2) 0.02425(9) Uani 1 1 d . . . . .
Cl1 Cl 0.12967(6) 0.22504(3) 0.75547(3) 0.03378(14) Uani 1 1 d . . . . .
N1 N 0.4774(2) 0.14781(11) 0.79194(12) 0.0320(4) Uani 1 1 d . . . . .
P1 P 0.44845(6) 0.18745(3) 0.70391(3) 0.02589(13) Uani 1 1 d . . . . .
C1 C 0.4265(2) 0.27730(12) 0.70702(13) 0.0266(5) Uani 1 1 d . . . . .
Cl2 Cl 0.30457(6) 0.36826(3) 0.84878(3) 0.03289(14) Uani 1 1 d . . . . .
C2 C 0.5021(3) 0.07153(14) 0.79977(15) 0.0381(6) Uani 1 1 d . . . . .
H2A H 0.536536 0.055537 0.756757 0.046 Uiso 1 1 calc R U . . .
H2AB H 0.416879 0.047733 0.796449 0.046 Uiso 1 1 calc R U . . .
N2 N 0.6725(2) 0.35324(11) 0.76038(11) 0.0305(4) Uani 1 1 d . . . . .
P2 P 0.54047(6) 0.33654(3) 0.68718(3) 0.02620(13) Uani 1 1 d . . . . .
Cl3 Cl 0.12939(6) 0.38009(3) 0.65095(3) 0.03312(14) Uani 1 1 d . . . . .
C3 C 0.5971(4) 0.04974(16) 0.87150(17) 0.0540(8) Uani 1 1 d . . . . .
H3A H 0.687628 0.063268 0.869385 0.065 Uiso 1 1 calc R U . . .
H3AB H 0.594963 -0.001426 0.875916 0.065 Uiso 1 1 calc R U . . .
C4 C 0.5653(3) 0.08239(15) 0.94147(15) 0.0417(6) Uani 1 1 d . . . . .
H4A H 0.484448 0.060829 0.950486 0.050 Uiso 1 1 calc R U . . .
H4AB H 0.638761 0.073259 0.986039 0.050 Uiso 1 1 calc R U . . .
C6 C 0.4488(3) 0.18074(14) 0.85991(15) 0.0367(6) Uani 1 1 d . . . . .
H6A H 0.358736 0.167491 0.863105 0.044 Uiso 1 1 calc R U . . .
H6AB H 0.450705 0.231810 0.854351 0.044 Uiso 1 1 calc R U . . .
C29 C 0.4391(3) 0.46456(13) 0.72033(15) 0.0340(5) Uani 1 1 d . . . . .
H29 H 0.460350 0.447421 0.770481 0.041 Uiso 1 1 calc R U . . .
C24 C 0.4636(2) 0.42261(13) 0.66095(14) 0.0306(5) Uani 1 1 d . . . . .
C23 C 0.6727(3) 0.33504(16) 0.84040(14) 0.0381(6) Uani 1 1 d . . . . .
H23A H 0.614264 0.294702 0.840959 0.046 Uiso 1 1 calc R U . . .
H23B H 0.638722 0.374678 0.864512 0.046 Uiso 1 1 calc R U . . .
C22 C 0.8138(3) 0.31753(17) 0.88456(17) 0.0447(7) Uani 1 1 d . . . . .
H22A H 0.844954 0.275821 0.862372 0.054 Uiso 1 1 calc R U . . .
H22B H 0.813654 0.306727 0.937450 0.054 Uiso 1 1 calc R U . . .
C21 C 0.9100(3) 0.37869(17) 0.88309(17) 0.0451(7) Uani 1 1 d . . . . .
H21A H 0.885189 0.418935 0.910358 0.054 Uiso 1 1 calc R U . . .
H21B H 1.001072 0.364754 0.908817 0.054 Uiso 1 1 calc R U . . .
C20 C 0.9047(3) 0.39951(17) 0.80054(17) 0.0447(7) Uani 1 1 d . . . . .
H20A H 0.941185 0.361418 0.775388 0.054 Uiso 1 1 calc R U . . .
H20B H 0.959755 0.441284 0.800142 0.054 Uiso 1 1 calc R U . . .
C30 C 0.6135(3) 0.31039(13) 0.60854(14) 0.0315(5) Uani 1 1 d . . . . .
C35 C 0.5309(3) 0.29961(14) 0.53524(15) 0.0352(6) Uani 1 1 d . . . . .
H35 H 0.437969 0.304493 0.526572 0.042 Uiso 1 1 calc R U . . .
C31 C 0.7521(3) 0.30017(16) 0.62076(17) 0.0425(6) Uani 1 1 d . . . . .
H31 H 0.807752 0.306889 0.669630 0.051 Uiso 1 1 calc R U . . .
C34 C 0.5889(3) 0.28140(15) 0.47489(15) 0.0428(7) Uani 1 1 d . . . . .
H34 H 0.534707 0.275923 0.425455 0.051 Uiso 1 1 calc R U . . .
C25 C 0.4322(3) 0.45008(15) 0.58649(16) 0.0388(6) Uani 1 1 d . . . . .
H25 H 0.447947 0.422987 0.546210 0.047 Uiso 1 1 calc R U . . .
C16 C 0.0961(3) 0.08944(14) 0.52287(15) 0.0389(6) Uani 1 1 d . . . . .
H16 H 0.026628 0.069804 0.485244 0.047 Uiso 1 1 calc R U . . .
C15 C 0.1833(3) 0.04629(15) 0.57353(18) 0.0493(7) Uani 1 1 d . . . . .
H15 H 0.171891 -0.002572 0.570232 0.059 Uiso 1 1 calc R U . . .
C14 C 0.2880(3) 0.07482(14) 0.62946(15) 0.0375(6) Uani 1 1 d . . . . .
H14 H 0.346422 0.045017 0.663247 0.045 Uiso 1 1 calc R U . . .
C13 C 0.3062(2) 0.14842(12) 0.63535(13) 0.0263(5) Uani 1 1 d . . . . .
C12 C 0.7183(3) 0.15737(17) 0.72597(18) 0.0435(7) Uani 1 1 d . . . . .
H12 H 0.727885 0.178514 0.773866 0.052 Uiso 1 1 calc R U . . .
C11 C 0.8275(3) 0.12621(18) 0.7071(2) 0.0592(9) Uani 1 1 d . . . . .
H11 H 0.908953 0.123320 0.743842 0.071 Uiso 1 1 calc R U . . .
C10 C 0.8178(3) 0.09908(19) 0.6343(2) 0.0596(9) Uani 1 1 d . . . . .
H10 H 0.893503 0.080467 0.621254 0.072 Uiso 1 1 calc R U . . .
C9 C 0.6938(4) 0.0998(2) 0.5805(2) 0.0630(9) Uani 1 1 d . . . . .
H9 H 0.685536 0.079186 0.532481 0.076 Uiso 1 1 calc R U . . .
C8 C 0.5838(3) 0.13094(16) 0.59816(16) 0.0420(6) Uani 1 1 d . . . . .
H8 H 0.503454 0.134667 0.560630 0.050 Uiso 1 1 calc R U . . .
C7 C 0.5917(2) 0.15722(13) 0.67249(14) 0.0289(5) Uani 1 1 d . . . . .
C28 C 0.3837(3) 0.53117(15) 0.70519(17) 0.0424(6) Uani 1 1 d . . . . .
H28 H 0.366268 0.558342 0.744977 0.051 Uiso 1 1 calc R U . . .
C18 C 0.2171(3) 0.19136(13) 0.58346(15) 0.0336(5) Uani 1 1 d . . . . .
H18 H 0.228148 0.240268 0.586038 0.040 Uiso 1 1 calc R U . . .
C19 C 0.7603(3) 0.41478(16) 0.75659(16) 0.0394(6) Uani 1 1 d . . . . .
H19A H 0.726966 0.455997 0.778499 0.047 Uiso 1 1 calc R U . . .
H19B H 0.758139 0.425137 0.703295 0.047 Uiso 1 1 calc R U . . .
C17 C 0.1122(3) 0.16233(14) 0.52809(15) 0.0347(5) Uani 1 1 d . . . . .
H17 H 0.052614 0.191721 0.494434 0.042 Uiso 1 1 calc R U . . .
C33 C 0.7266(3) 0.27149(17) 0.48829(18) 0.0491(7) Uani 1 1 d . . . . .
H33 H 0.764342 0.258897 0.447921 0.059 Uiso 1 1 calc R U . . .
C5 C 0.5447(4) 0.16041(16) 0.93145(16) 0.0488(7) Uani 1 1 d . . . . .
H5A H 0.513050 0.178730 0.974490 0.059 Uiso 1 1 calc R U . . .
H5AB H 0.630860 0.182520 0.932827 0.059 Uiso 1 1 calc R U . . .
C27 C 0.3540(3) 0.55760(16) 0.63129(19) 0.0489(7) Uani 1 1 d . . . . .
H27 H 0.317653 0.602782 0.621477 0.059 Uiso 1 1 calc R U . . .
C32 C 0.8078(3) 0.28013(19) 0.56088(18) 0.0510(8) Uani 1 1 d . . . . .
H32 H 0.900087 0.272512 0.569807 0.061 Uiso 1 1 calc R U . . .
C26 C 0.3779(3) 0.51730(16) 0.57198(18) 0.0488(7) Uani 1 1 d . . . . .
H26 H 0.357673 0.535239 0.522159 0.059 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 0.0181 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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga -1.2846 0.7763 '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'
P P 0.2955 0.4335 '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
C1 Ga1 Cl3 115.61(7) . . ?
C1 Ga1 Cl1 112.66(7) . . ?
Cl3 Ga1 Cl1 104.04(3) . . ?
C1 Ga1 Cl2 113.92(7) . . ?
Cl3 Ga1 Cl2 107.62(2) . . ?
Cl1 Ga1 Cl2 101.65(2) . . ?
C6 N1 C2 113.9(2) . . ?
C6 N1 P1 124.07(17) . . ?
C2 N1 P1 120.51(17) . . ?
N1 P1 C1 113.51(11) . . ?
N1 P1 C7 100.36(11) . . ?
C1 P1 C7 116.77(11) . . ?
N1 P1 C13 112.23(11) . . ?
C1 P1 C13 109.49(11) . . ?
C7 P1 C13 103.92(11) . . ?
P2 C1 P1 122.56(13) . . ?
P2 C1 Ga1 119.93(12) . . ?
P1 C1 Ga1 117.51(12) . . ?
N1 C2 C3 114.9(2) . . ?
C23 N2 C19 111.7(2) . . ?
C23 N2 P2 122.08(17) . . ?
C19 N2 P2 119.78(17) . . ?
N2 P2 C1 114.94(11) . . ?
N2 P2 C30 104.74(11) . . ?
C1 P2 C30 114.35(11) . . ?
N2 P2 C24 104.55(11) . . ?
C1 P2 C24 111.34(11) . . ?
C30 P2 C24 106.03(11) . . ?
C2 C3 C4 112.6(3) . . ?
C5 C4 C3 110.9(2) . . ?
N1 C6 C5 113.1(2) . . ?
C28 C29 C24 120.5(3) . . ?
C25 C24 C29 118.4(2) . . ?
C25 C24 P2 124.4(2) . . ?
C29 C24 P2 117.15(19) . . ?
N2 C23 C22 109.8(2) . . ?
C23 C22 C21 111.5(2) . . ?
C20 C21 C22 110.1(2) . . ?
C21 C20 C19 110.7(2) . . ?
C35 C30 C31 119.2(2) . . ?
C35 C30 P2 120.09(19) . . ?
C31 C30 P2 120.7(2) . . ?
C30 C35 C34 119.4(3) . . ?
C32 C31 C30 120.6(3) . . ?
C33 C34 C35 120.3(3) . . ?
C26 C25 C24 120.6(3) . . ?
C15 C16 C17 119.8(3) . . ?
C16 C15 C14 120.7(3) . . ?
C15 C14 C13 120.3(2) . . ?
C18 C13 C14 118.2(2) . . ?
C18 C13 P1 120.15(19) . . ?
C14 C13 P1 121.51(19) . . ?
C11 C12 C7 119.9(3) . . ?
C12 C11 C10 121.0(3) . . ?
C11 C10 C9 119.5(3) . . ?
C8 C9 C10 120.3(3) . . ?
C9 C8 C7 120.5(3) . . ?
C8 C7 C12 118.4(2) . . ?
C8 C7 P1 123.3(2) . . ?
C12 C7 P1 118.2(2) . . ?
C27 C28 C29 120.2(3) . . ?
C17 C18 C13 121.0(2) . . ?
N2 C19 C20 110.5(2) . . ?
C18 C17 C16 120.0(2) . . ?
C32 C33 C34 120.3(2) . . ?
C6 C5 C4 114.2(3) . . ?
C26 C27 C28 120.2(3) . . ?
C33 C32 C31 120.0(3) . . ?
C27 C26 C25 120.0(3) . . ?
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 C1 1.986(2) . ?
Ga1 Cl3 2.1953(6) . ?
Ga1 Cl1 2.2133(6) . ?
Ga1 Cl2 2.2286(6) . ?
N1 C6 1.459(3) . ?
N1 C2 1.463(3) . ?
N1 P1 1.706(2) . ?
P1 C1 1.714(2) . ?
P1 C7 1.786(2) . ?
P1 C13 1.817(2) . ?
C1 P2 1.714(2) . ?
C2 C3 1.469(4) . ?
N2 C23 1.474(3) . ?
N2 C19 1.480(3) . ?
N2 P2 1.668(2) . ?
P2 C30 1.817(2) . ?
P2 C24 1.817(3) . ?
C3 C4 1.502(4) . ?
C4 C5 1.493(4) . ?
C6 C5 1.464(4) . ?
C29 C28 1.379(4) . ?
C29 C24 1.397(4) . ?
C24 C25 1.395(4) . ?
C23 C22 1.505(4) . ?
C22 C21 1.521(4) . ?
C21 C20 1.519(4) . ?
C20 C19 1.524(4) . ?
C30 C35 1.394(4) . ?
C30 C31 1.395(4) . ?
C35 C34 1.397(4) . ?
C31 C32 1.384(4) . ?
C34 C33 1.382(4) . ?
C25 C26 1.385(4) . ?
C16 C15 1.375(4) . ?
C16 C17 1.386(4) . ?
C15 C14 1.386(4) . ?
C14 C13 1.403(3) . ?
C13 C18 1.394(4) . ?
C12 C11 1.375(4) . ?
C12 C7 1.412(4) . ?
C11 C10 1.383(5) . ?
C10 C9 1.395(5) . ?
C9 C8 1.372(4) . ?
C8 C7 1.405(4) . ?
C28 C27 1.378(4) . ?
C18 C17 1.385(4) . ?
C33 C32 1.373(4) . ?
C27 C26 1.377(4) . ?
