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_7120317
_publ_section_title
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 An NHC--phosphinidenyl as a synthon for new group 13/15 compounds
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_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC04422D
_journal_year                    2017
_chemical_formula_moiety         'C37 H62 Cl Ga2 N2 P'
_chemical_formula_sum            'C37 H62 Cl Ga2 N2 P'
_chemical_formula_weight         740.74
_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             2016-05-17
_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                84.726(2)
_cell_angle_beta                 83.754(2)
_cell_angle_gamma                61.541(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7012(6)
_cell_length_b                   9.8809(4)
_cell_length_c                   23.0792(12)
_cell_measurement_reflns_used    9686
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.122
_cell_measurement_theta_min      2.347
_cell_volume                     1931.38(18)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.882
_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  0.0389
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            81566
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.939
_diffrn_reflns_theta_min         2.347
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.532
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1219 before and 0.0485 after correction.
The Ratio of minimum to maximum transmission is 0.8535.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.278
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         11774
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0190P)^2^+1.4860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9701
_reflns_number_total             11774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc04422d2.cif
_cod_data_source_block           ol440_0m
_cod_database_code               7120317
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C6(H6), C8(H8), C15(H15)
2.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C36(H36A,H36B,
 H36C), C19(H19A,H19B,H19C), C10(H10A,H10B,H10C), C35(H35A,H35B,H35C), C33(H33A,
 H33B,H33C), C32(H32A,H32B,H32C), C37(H37A,H37B,H37C), C24(H24A,H24B,H24C),
 C25(H25A,H25B,H25C), C29(H29A,H29B,H29C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              9806
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'