Crystalline phosphino(silyl)carbenes that readily form transition metal complexes
Löwe, Pawel; Dielmann, Fabian; Chemical Communications  (2022) –; doi:10.1039/D2CC04321A

data_7130802
_publ_section_title
;
 Crystalline phosphino(silyl)carbenes that readily form transition metal
 complexes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04321A
_journal_year                    2022
_chemical_formula_moiety         'Cl, C22 H40 N6 P'
_chemical_formula_sum            'C22 H40 Cl N6 P'
_chemical_formula_weight         455.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_audit_update_record
;
2022-09-27 deposited with the CCDC.	2022-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                66.9530(10)
_cell_angle_beta                 81.9680(10)
_cell_angle_gamma                84.7670(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3440(2)
_cell_length_b                   10.8041(2)
_cell_length_c                   12.4387(2)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.72
_cell_volume                     1265.60(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0173
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19793
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.277
_diffrn_reflns_theta_min         1.791
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1385 before and 0.0288 after correction. The Ratio of minimum to maximum transmission is 0.9223. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       block
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.576
_exptl_crystal_size_min          0.432
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         6269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.5130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5847
_reflns_number_total             6269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04321a2.cif
_cod_data_source_block           tw170804_0m_a
_cod_database_code               7130802
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6(0.016) H5(0.016) H4(0.019) H17A(0.026) H17B(0.026) H17C(0.026)
 H3(0.019) H15A(0.027) H15B(0.027) H15C(0.027) H22A(0.026) H22B(0.026)
 H22C(0.026) H11A(0.028) H11B(0.028) H11C(0.028) H14A(0.029) H14B(0.029)
 H14C(0.029) H19A(0.027) H19B(0.027) H19C(0.027) H20A(0.028) H20B(0.028)
 H20C(0.028) H18A(0.031) H18B(0.031) H18C(0.031) H13A(0.032) H13B(0.032)
 H13C(0.032) H16A(0.028) H16B(0.028) H16C(0.028) H21A(0.03) H21B(0.03)
 H21C(0.03) H12A(0.032) H12B(0.032) H12C(0.032)
 Fixed X: H6(0.5902) H5(0.6301) H4(0.7318) H17A(0.9578) H17B(0.9222)
 H17C(0.8881) H3(0.7747) H15A(0.6469) H15B(0.6378) H15C(0.5688) H22A(0.4887)
 H22B(0.5663) H22C(0.5915) H11A(0.9559) H11B(0.9208) H11C(0.8099) H14A(0.9705)
 H14B(0.8929) H14C(0.8938) H19A(0.6472) H19B(0.679) H19C(0.5714) H20A(0.8308)
 H20B(0.8119) H20C(0.8822) H18A(0.6862) H18B(0.8029) H18C(0.8341) H13A(0.6645)
 H13B(0.7646) H13C(0.718) H16A(0.6855) H16B(0.7714) H16C(0.8415) H21A(0.7235)
 H21B(0.6527) H21C(0.5698) H12A(0.9554) H12B(1.0088) H12C(1.0451)
 Fixed Y: H6(0.3221) H5(0.565) H4(0.3073) H17A(0.608) H17B(0.7441)
 H17C(0.6018) H3(0.5487) H15A(0.1846) H15B(0.0389) H15C(0.1676) H22A(0.1738)
 H22B(0.041) H22C(0.1836) H11A(0.6882) H11B(0.8251) H11C(0.7518) H14A(0.1363)
 H14B(0.019) H14C(0.1652) H19A(0.6646) H19B(0.8124) H19C(0.7282) H20A(0.157)
 H20B(0.0135) H20C(0.1294) H18A(0.7609) H18B(0.8382) H18C(0.7064) H13A(0.7343)
 H13B(0.8181) H13C(0.676) H16A(0.0987) H16B(-0.0197) H16C(0.0986) H21A(0.101)
 H21B(-0.0119) H21C(0.1158) H12A(0.5949) H12B(0.7305) H12C(0.5886)
 Fixed Z: H6(0.9035) H5(0.8096) H4(0.0427) H17A(0.5659) H17B(0.4595)
 H17C(0.4611) H3(-0.0386) H15A(0.4193) H15B(0.4163) H15C(0.3239) H22A(0.7368)
 H22B(0.731) H22C(0.6252) H11A(-0.0493) H11B(-0.0286) H11C(-0.0568)
 H14A(0.2882) H14B(0.3937) H14C(0.3975) H19A(0.4515) H19B(0.4384) H19C(0.5403)
 H20A(0.6429) H20B(0.7488) H20C(0.7661) H18A(0.687) H18B(0.5921) H18C(0.7041)
 H13A(0.1208) H13B(0.1502) H13C(0.2467) H16A(0.1695) H16B(0.2557) H16C(0.1453)
 H21A(0.9427) H21B(0.9216) H21C(0.9329) H12A(0.262) H12B(0.1597) H12C(0.1483)
;
_shelx_res_checksum              91814
_shelx_hkl_checksum              15942
_olex2_submission_original_sample_id tw212
_olex2_submission_special_instructions 'No special instructions were received'