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

data_7130806
_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         'C32 H52 Cu F2 N6 P Si'
_chemical_formula_sum            'C32 H52 Cu F2 N6 P Si'
_chemical_formula_weight         681.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-05
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0953(8)
_cell_length_b                   10.1679(4)
_cell_length_c                   17.1211(7)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      2.24
_cell_volume                     3498.3(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.991
_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  0.0591
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45781
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.115
_diffrn_reflns_theta_min         2.027
_diffrn_source_current           0.59
_diffrn_source_power             0.0295
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1337 before and 0.0684 after correction.
The Ratio of minimum to maximum transmission is 0.8076.
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    1.294
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_preparation       'PL540 procedure'
_exptl_crystal_recrystallization_method
'cristallized by diffusion of n-hexane into a saturated difluorobenzene solution over 4 months'
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.116
_refine_diff_density_max         1.559
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Flack x determined using 3560 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.012(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         9272
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0790P)^2^+0.0988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1285
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                8247
_reflns_number_total             9272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04321a2.cif
_cod_data_source_block           pna21_a
_cod_database_code               7130806
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.594
_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), C32(H32), C3(H3), C4(H4), C31(H31), C30(H30)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C26(H26A,H26B,H26C), C11(H11A,H11B,H11C), C21(H21A,H21B,
 H21C), C24(H24A,H24B,H24C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C18(H18A,
 H18B,H18C), C8(H8A,H8B,H8C), C25(H25A,H25B,H25C), C23(H23A,H23B,H23C),
 C22(H22A,H22B,H22C), C6(H6A,H6B,H6C), C17(H17A,H17B,H17C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              28800
_shelx_hkl_checksum              26144
_olex2_date_sample_submission    2021-01-04
_olex2_exptl_crystal_mounting_method 'mounted on a glass capillarry'
_olex2_submission_original_sample_id PL540
_olex2_submission_special_instructions 'No special instructions were received'