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

data_7130807
_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, 2(C11 H22 N3 P0.5), 2(C6 H5 F)'
_chemical_formula_sum            'C34 H54 Cl F2 N6 P'
_chemical_formula_weight         651.25
_chemical_name_systematic        (sItBuN)2PCl
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-09-27 deposited with the CCDC.	2022-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.9270(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.3923(6)
_cell_length_b                   5.86980(10)
_cell_length_c                   26.0141(6)
_cell_measurement_reflns_used    9519
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      2.28
_cell_volume                     3593.12(14)
_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      100.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0401
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            54469
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.605
_diffrn_reflns_theta_min         2.387
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0767 before and 0.0507 after correction.
The Ratio of minimum to maximum transmission is 0.8527.
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    1.204
_exptl_crystal_description       needle
_exptl_crystal_F_000             1400
_exptl_crystal_preparation       'via EXP PL787'
_exptl_crystal_recrystallization_method
'crystallized by cooling down a saturated solution of fluorobenzene'
_exptl_crystal_size_max          0.487
_exptl_crystal_size_mid          0.458
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         10031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0644P)^2^+0.9960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1238
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9609
_reflns_number_total             10031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04321a2.cif
_cod_data_source_block           p21c_a
_cod_original_cell_volume        3593.12(13)
_cod_database_code               7130807
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.912
_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. Others
 Fixed Sof: P1B(0.5) P1A(0.5) N1B(0.5) N4B(0.5) N4A(0.5) N1A(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C2(H2A,H2B), C3(H3A,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C24(H24), C34(H34), C26(H26), C27(H27), C30(H30), C31(H31),
 C25(H25), C32(H32), C33(H33)
3.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C17(H17A,H17B,H17C), C12(H12A,H12B,H12C), C16(H16A,H16B,
 H16C), C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C10(H10A,
 H10B,H10C), C13(H13A,H13B,H13C), C22(H22A,H22B,H22C), C9(H9A,H9B,H9C),
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              44558
_shelx_hkl_checksum              54060
_olex2_date_sample_data_collection 2022-03-03
_olex2_date_sample_submission    2022-03-03
_olex2_exptl_crystal_mounting_method 'mounted on glass capillary'
_olex2_submission_original_sample_id PL787
_olex2_submission_special_instructions 'No special instructions were received'