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

data_7130805
_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         'C26 H53 N6 P Si'
_chemical_formula_sum            'C26 H53 N6 P Si'
_chemical_formula_weight         508.80
_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     dual
_audit_creation_date             2020-05-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2022-09-27 deposited with the CCDC.	2022-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                79.803(3)
_cell_angle_beta                 73.474(3)
_cell_angle_gamma                78.577(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0192(5)
_cell_length_b                   11.9241(5)
_cell_length_c                   12.4677(5)
_cell_measurement_reflns_used    7132
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.44
_cell_measurement_theta_min      2.29
_cell_volume                     1526.65(12)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_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  0.0437
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.987
_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       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24627
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.593
_diffrn_reflns_theta_min         1.718
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.153
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0897 before and 0.0486 after correction.
The Ratio of minimum to maximum transmission is 0.8618.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.167
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         8484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0787P)^2^+0.9776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6578
_reflns_number_total             8484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04321a2.cif
_cod_data_source_block           p-1_a_CCDC1
_cod_database_code               7130805
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.961
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C3(H3A,H3B), C4(H4A,H4B)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C21(H21A,H21B,H21C), C12(H12A,H12B,
 H12C), C11(H11A,H11B,H11C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C19(H19A,
 H19B,H19C), C25(H25A,H25B,H25C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C18(H18A,
 H18B,H18C), C17(H17A,H17B,H17C), C10(H10A,H10B,H10C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              89909
_shelx_hkl_checksum              4962
_olex2_date_sample_data_collection 2020-05-16
_olex2_date_sample_submission    2020-05-15
_olex2_submission_original_sample_id PL432
_olex2_submission_special_instructions 'No special instructions were received'