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

data_7130808
_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         'C34 H67 Cu2 N6 O2 P Si, C6 H6'
_chemical_formula_sum            'C40 H73 Cu2 N6 O2 P Si'
_chemical_formula_weight         856.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-09-27 deposited with the CCDC.	2022-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.6481(9)
_cell_length_b                   18.7415(8)
_cell_length_c                   22.4951(9)
_cell_measurement_reflns_used    9775
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.70
_cell_measurement_theta_min      2.31
_cell_volume                     9126.7(7)
_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, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_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  0.0626
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            131767
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.312
_diffrn_reflns_theta_min         1.699
_exptl_absorpt_coefficient_mu    1.032
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0920 before and 0.0616 after correction.
The Ratio of minimum to maximum transmission is 0.7482.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       block
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.528
_exptl_crystal_size_mid          0.524
_exptl_crystal_size_min          0.165
_refine_diff_density_max         2.240
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         11234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+21.3699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9127
_reflns_number_total             11234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04321a2.cif
_cod_data_source_block           pbca_a
_cod_database_code               7130808
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.612
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C4(H4), C3(H3), C38(H38), C37(H37), C35(H35), C40(H40),
 C36(H36), C39(H39)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C24(H24A,H24B,
 H24C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C19(H19A,
 H19B,H19C), C17(H17A,H17B,H17C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C26(H26A,
 H26B,H26C), C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C10(H10A,H10B,H10C),
 C18(H18A,H18B,H18C), C8(H8A,H8B,H8C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C),
  C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              65989
_shelx_hkl_checksum              64346
_olex2_submission_special_instructions 'No special instructions were received'