An NHC‒phosphinidenyl as a synthon for new group 13/15 compounds
Lemp, Otfried; Balmer, Markus; Reiter, Kevin; Weigend, Florian; von Hänisch, Carsten; Chem. Commun.  (2017) –; doi:10.1039/C7CC04422D

data_7120322
_publ_section_title
;
 An NHC--phosphinidenyl as a synthon for new group 13/15 compounds
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04422D
_journal_year                    2017
_chemical_formula_moiety         'C58 H88 Ga2 N4 P2'
_chemical_formula_sum            'C58 H88 Ga2 N4 P2'
_chemical_formula_weight         1042.70
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-03-10 deposited with the CCDC.
2017-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                100.545(2)
_cell_angle_beta                 101.098(2)
_cell_angle_gamma                106.378(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8600(6)
_cell_length_b                   12.9739(7)
_cell_length_c                   22.3682(12)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      19.928
_cell_measurement_theta_min      2.297
_cell_volume                     3135.8(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            78201
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.061
_diffrn_reflns_theta_min         2.144
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0967 before and 0.0593 after correction.
The Ratio of minimum to maximum transmission is 0.9093.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.155
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         13720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0434
_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/[\s^2^(Fo^2^)+(0.0430P)^2^+1.3870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9707
_reflns_number_total             13720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04422d2.cif
_cod_data_source_block           ol389_0m
_cod_database_code               7120322
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.709
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H29(0.025) H58A(0.032) H58B(0.032) H58C(0.032) H27(0.025)
 H56A(0.034) H56B(0.034) H56C(0.034) H50A(0.039) H50B(0.039) H50C(0.039)
 H53A(0.039) H53B(0.039) H53C(0.039) H57A(0.035) H57B(0.035) H57C(0.035)
 H54A(0.036) H54B(0.036) H54C(0.036) H2A(0.026) H2B(0.026) H52A(0.036)
 H52B(0.036) H52C(0.036) H31A(0.037) H31B(0.037) H31C(0.037) H19A(0.039)
 H19B(0.039) H19C(0.039) H33A(0.039) H33B(0.039) H33C(0.039) H46A(0.046)
 H46B(0.046) H46C(0.046) H10A(0.039) H10B(0.039) H10C(0.039) H44A(0.042)
 H44B(0.042) H44C(0.042) H6(0.033) H12A(0.041) H12B(0.041) H12C(0.041)
 H48A(0.04) H48B(0.04) H48C(0.04) H49A(0.038) H49B(0.038) H49C(0.038)
 H36(0.033) H38(0.033) H3A(0.033) H3B(0.033) H15(0.033) H40A(0.044) H40B(0.044)
 H40C(0.044) H42A(0.049) H42B(0.049) H42C(0.049) H45A(0.05) H45B(0.05)
 H45C(0.05) H8(0.033) H21A(0.047) H21B(0.047) H21C(0.047) H32A(0.048)
 H32B(0.048) H32C(0.048) H17(0.037) H23A(0.039) H23B(0.039) H41A(0.061)
 H41B(0.061) H41C(0.061) H24A(0.039) H24B(0.039) H20A(0.068) H20B(0.068)
 H20C(0.068) H11A(0.075) H11B(0.075) H11C(0.075)
 Fixed X: H29(1.1808) H58A(1.1445) H58B(1.1421) H58C(1.0308) H27(0.9763)
 H56A(1.0874) H56B(1.1753) H56C(1.1797) H50A(0.3904) H50B(0.4317) H50C(0.5212)
 H53A(1.1141) H53B(1.1625) H53C(1.1815) H57A(0.8906) H57B(1.0095) H57C(0.9212)
 H54A(0.8434) H54B(0.9603) H54C(0.9111) H2A(0.9194) H2B(0.9619) H52A(1.0796)
 H52B(1.0688) H52C(0.9503) H31A(0.7408) H31B(0.7666) H31C(0.7) H19A(0.8506)
 H19B(0.8499) H19C(0.8814) H33A(1.1097) H33B(0.9728) H33C(1.001) H46A(0.5808)
 H46B(0.4449) H46C(0.509) H10A(1.1418) H10B(1.2096) H10C(1.108) H44A(0.3906)
 H44B(0.3635) H44C(0.4983) H6(1.1533) H12A(0.66) H12B(0.6468) H12C(0.6743)
 H48A(0.4498) H48B(0.3923) H48C(0.3462) H49A(0.681) H49B(0.5854) H49C(0.6517)
 H36(0.2421) H38(0.5273) H3A(0.7822) H3B(0.7221) H15(0.6559) H40A(0.3427)
 H40B(0.2739) H40C(0.4087) H42A(0.7521) H42B(0.7231) H42C(0.7466) H45A(0.3484)
 H45B(0.2747) H45C(0.2976) H8(0.804) H21A(0.4949) H21B(0.3921) H21C(0.5199)
 H32A(1.2666) H32B(1.1761) H32C(1.2336) H17(0.3777) H23A(0.7685) H23B(0.7769)
 H41A(0.203) H41B(0.3094) H41C(0.2937) H24A(0.5718) H24B(0.5759) H20A(0.3718)
 H20B(0.3692) H20C(0.4719) H11A(1.0191) H11B(0.9669) H11C(1.1056)
 Fixed Y: H29(0.3536) H58A(0.858) H58B(0.8465) H58C(0.8674) H27(0.3895)
 H56A(0.5691) H56B(0.6608) H56C(0.681) H50A(0.3932) H50B(0.3922) H50C(0.3844)
 H53A(0.8501) H53B(0.7821) H53C(0.7656) H57A(0.6953) H57B(0.6854) H57C(0.582)
 H54A(0.6445) H54B(0.7019) H54C(0.7757) H2A(1.1513) H2B(1.1063) H52A(0.5638)
 H52B(0.5788) H52C(0.5147) H31A(0.4161) H31B(0.3453) H31C(0.2837) H19A(0.8497)
 H19B(0.8818) H19C(0.9768) H33A(0.3496) H33B(0.3438) H33C(0.2342) H46A(0.6581)
 H46B(0.615) H46C(0.5277) H10A(1.1394) H10B(1.0584) H10C(1.0153) H44A(0.7091)
 H44B(0.7143) H44C(0.7724) H6(1.0553) H12A(0.841) H12B(0.9314) H12C(0.964)
 H48A(0.6754) H48B(0.5743) H48C(0.5657) H49A(0.5487) H49B(0.5529) H49C(0.6611)
 H36(0.237) H38(0.379) H3A(1.1151) H3B(1.0994) H15(0.8383) H40A(0.1323)
 H40B(0.2215) H40C(0.248) H42A(0.4558) H42B(0.3868) H42C(0.3288) H45A(0.4342)
 H45B(0.51) H45C(0.5075) H8(0.9454) H21A(1.0339) H21B(0.9148) H21C(0.9387)
 H32A(0.3738) H32B(0.3482) H32C(0.4726) H17(0.8834) H23A(0.1504) H23B(0.1921)
 H41A(0.2777) H41B(0.2921) H41C(0.399) H24A(0.1296) H24B(0.1516) H20A(0.7355)
 H20B(0.8589) H20C(0.8201) H11A(1.0746) H11B(0.942) H11C(1.0028)
 Fixed Z: H29(0.8234) H58A(0.8775) H58B(0.9473) H58C(0.904) H27(0.9448)
 H56A(0.8577) H56B(0.9196) H56C(0.8515) H50A(0.7916) H50B(0.8638) H50C(0.8193)
 H53A(0.7552) H53B(0.7045) H53C(0.7745) H57A(0.9229) H57B(0.9661) H57C(0.9099)
 H54A(0.6517) H54B(0.6291) H54C(0.6765) H2A(0.8347) H2B(0.895) H52A(0.7362)
 H52B(0.6661) H52C(0.6855) H31A(0.8612) H31B(0.9106) H31C(0.8382) H19A(0.9417)
 H19B(1.0141) H19C(0.9775) H33A(0.7155) H33B(0.6874) H33C(0.6983) H46A(0.654)
 H46B(0.6099) H46C(0.628) H10A(0.8393) H10B(0.8118) H10C(0.8475) H44A(0.7563)
 H44B(0.6842) H44C(0.7292) H6(0.7034) H12A(0.6925) H12B(0.654) H12C(0.7291)
 H48A(0.8687) H48B(0.8972) H48C(0.8237) H49A(0.8992) H49B(0.9405) H49C(0.9197)
 H36(0.5638) H38(0.5008) H3A(0.9123) H3B(0.8387) H15(1.0299) H40A(0.6627)
 H40B(0.6722) H40C(0.7146) H42A(0.6183) H42B(0.5469) H42C(0.6032) H45A(0.6749)
 H45B(0.6491) H45C(0.7216) H8(0.6049) H21A(0.8423) H21B(0.8133) H21C(0.7956)
 H32A(0.9311) H32B(0.9752) H32C(0.97) H17(0.9157) H23A(0.7267) H23B(0.6635)
 H41A(0.4646) H41B(0.4292) H41C(0.4707) H24A(0.644) H24B(0.7179) H20A(1.0006)
 H20B(1.0235) H20C(1.0614) H11A(0.5741) H11B(0.5504) H11C(0.5899)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'