[((Cl)Im(Dipp))P[double bond, length as m-dash]P(Dipp)][GaCl4]: a polarized, cationic diphosphene.
Schwedtmann, Kai; Holthausen, Michael H.; Sala, Chris H.; Hennersdorf, Felix; Fröhlich, Roland; Weigand, Jan J.; Chemical communications (Cambridge, England) 52 (2016) 1409–1412; doi:10.1039/c5cc08248j

data_7118451
_publ_section_title
;
 [((Cl)Im(Dipp))P[double bond, length as m-dash]P(Dipp)][GaCl4]: a
 polarized, cationic diphosphene.
;
_journal_issue                   7
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1409
_journal_page_last               1412
_journal_paper_doi               10.1039/c5cc08248j
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety
'C40 H54 Cl3 N2 P2, C6 H3 F2, C F3, O3 S, C6 H4 F2'
_chemical_formula_sum            'C53 H61 Cl3 F7 N2 O3 P2 S'
_chemical_formula_weight         1107.39
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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
;
2015-09-30 deposited with the CCDC.
2015-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.2620(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2639(2)
_cell_length_b                   12.5384(2)
_cell_length_c                   36.3192(7)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1
_cell_volume                     5511.98(17)
_computing_cell_refinement       'APEX2 Software Suit (v2012.2-0)'
_computing_data_collection       'APEX2 Software Suit (v2012.2-0)'
_computing_data_reduction        'APEX2 Software Suit (v2012.2-0)'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_solution
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  'HELIOS multilayer optics, Montel mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            54790
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.14
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.329
_exptl_absorpt_correction_T_max  0.9523
_exptl_absorpt_correction_T_min  0.8880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax = 0.9112  
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2308
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         13138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1055P)^2^+0.9597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1833
_reflns_number_gt                9459
_reflns_number_total             13138
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc08248j2.cif
_cod_data_source_block           added_by_encifer
_cod_original_cell_volume        5511.98(16)
_cod_database_code               7118451
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H4A(0.047) H4B(0.047) H4C(0.047) H7(0.047) H8(0.054) H9(0.046)
 H11(0.04) H12A(0.078) H12B(0.078) H12C(0.078) H13A(0.074) H13B(0.074)
 H13C(0.074) H14(0.037) H15A(0.068) H15B(0.068) H15C(0.068) H16A(0.064)
 H16B(0.064) H16C(0.064) H19(0.035) H20(0.039) H21(0.038) H23(0.033)
 H24A(0.062) H24B(0.062) H24C(0.062) H25A(0.053) H25B(0.053) H25C(0.053)
 H26(0.036) H27A(0.065) H27B(0.065) H27C(0.065) H28A(0.059) H28B(0.059)
 H28C(0.059) H31(0.047) H32(0.05) H33(0.044) H35(0.041) H36A(0.092) H36B(0.092)
 H36C(0.092) H37A(0.093) H37B(0.093) H37C(0.093) H38(0.043) H39A(0.081)
 H39B(0.081) H39C(0.081) H40A(0.08) H40B(0.08) H40C(0.08) H44(0.068) H45(0.071)
 H46(0.076) H50(0.081) H51(0.075) H52(0.089) H53(0.097)
 Fixed X: H4A(0.9067) H4B(1.005) H4C(1.0305) H7(1.0988) H8(1.267) H9(1.3239)
 H11(0.9007) H12A(0.9826) H12B(0.8743) H12C(0.9934) H13A(0.8511) H13B(0.7912)
 H13C(0.8982) H14(1.1646) H15A(1.3306) H15B(1.2841) H15C(1.2059) H16A(1.2941)
 H16B(1.3422) H16C(1.3835) H19(0.5086) H20(0.4992) H21(0.6578) H23(0.7505)
 H24A(0.7304) H24B(0.6781) H24C(0.5993) H25A(0.5153) H25B(0.6015) H25C(0.5856)
 H26(0.9328) H27A(0.7916) H27B(0.9216) H27C(0.8391) H28A(0.8945) H28B(0.9507)
 H28C(0.8203) H31(0.6958) H32(0.8043) H33(0.9176) H35(0.6895) H36A(0.7491)
 H36B(0.6313) H36C(0.6387) H37A(0.4982) H37B(0.5428) H37C(0.52) H38(0.9525)
 H39A(1.0872) H39B(1.1281) H39C(1.0907) H40A(0.8545) H40B(0.981) H40C(0.9402)
 H44(0.3532) H45(0.3703) H46(0.5217) H50(0.3335) H51(0.2705) H52(0.3451)
 H53(0.4782)
 Fixed Y: H4A(0.5619) H4B(0.5887) H4C(0.5732) H7(1.1325) H8(1.0951) H9(0.9203)
 H11(0.938) H12A(1.1445) H12B(1.0908) H12C(1.0406) H13A(1.0096) H13B(1.0771)
 H13C(1.1241) H14(0.6872) H15A(0.7533) H15B(0.6345) H15C(0.727) H16A(0.7296)
 H16B(0.6391) H16C(0.7598) H19(0.6778) H20(0.4934) H21(0.3913) H23(0.8358)
 H24A(0.8099) H24B(0.9219) H24C(0.8222) H25A(0.8538) H25B(0.9438) H25C(0.8393)
 H26(0.4886) H27A(0.3285) H27B(0.3387) H27C(0.4275) H28A(0.4032) H28B(0.3209)
 H28C(0.3164) H31(0.4903) H32(0.559) H33(0.7048) H35(0.575) H36A(0.4058)
 H36B(0.3998) H36C(0.3987) H37A(0.5539) H37B(0.6646) H37C(0.5664) H38(0.8453)
 H39A(0.7634) H39B(0.8377) H39C(0.7175) H40A(0.9343) H40B(0.9713) H40C(0.8885)
 H44(0.2357) H45(0.2791) H46(0.2171) H50(0.1687) H51(-0.0009) H52(-0.0945) H53(-
 0.0175)
 Fixed Z: H4A(0.9192) H4B(0.9525) H4C(0.911) H7(0.8654) H8(0.9019) H9(0.9138)
 H11(0.8237) H12A(0.8088) H12B(0.7857) H12C(0.784) H13A(0.8782) H13B(0.8433)
 H13C(0.8693) H14(0.8817) H15A(0.9419) H15B(0.9352) H15C(0.9466) H16A(0.8425)
 H16B(0.8718) H16C(0.8782) H19(0.8391) H20(0.8428) H21(0.8454) H23(0.8503)
 H24A(0.785) H24B(0.7941) H24C(0.7815) H25A(0.8378) H25B(0.8547) H25C(0.8786)
 H26(0.844) H27A(0.8052) H27B(0.805) H27C(0.7849) H28A(0.8988) H28B(0.8739)
 H28C(0.874) H31(1.0156) H32(1.0681) H33(1.0636) H35(0.9221) H36A(0.9479)
 H36B(0.9216) H36C(0.966) H37A(0.923) H37B(0.9415) H37C(0.9674) H38(0.9815)
 H39A(1.047) H39B(1.0161) H39C(1.0061) H40A(1.0239) H40B(1.0298) H40C(1.0582)
 H44(0.9784) H45(0.9171) H46(0.8916) H50(0.8319) H51(0.8145) H52(0.7698)
 H53(0.74)
;