Synthesis and properties of [PCP] pincer silylene cobalt(i) complexes
Li, Yonghui; Fan, Qingqing; Yang, Haiquan; Xie, Shangqing; Huang, Wei; Li, Xiaoyan; Sun, Hongjian; Fuhr, Olaf; Fenske, Dieter; New Journal of Chemistry 45 (2021) 19950–19956; doi:10.1039/D1NJ02982G

data_7060978
_publ_section_title
;
 Synthesis and properties of [PCP] pincer silylene cobalt(i) complexes
;
_journal_issue                   42
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19950
_journal_page_last               19956
_journal_paper_doi               10.1039/D1NJ02982G
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C45 H57 Cl Co N2 O2 P3 Si'
_chemical_formula_sum            'C45 H57 Cl Co N2 O2 P3 Si'
_chemical_formula_weight         873.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-26
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_audit_update_record
;
2021-09-14 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.478(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1744(3)
_cell_length_b                   9.3902(2)
_cell_length_c                   46.7097(14)
_cell_measurement_reflns_used    33542
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      64.38
_cell_measurement_theta_min      3.82
_cell_volume                     4449.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            25053
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         62.499
_diffrn_reflns_theta_min         3.817
_exptl_absorpt_coefficient_mu    3.468
_exptl_absorpt_correction_T_max  0.2776
_exptl_absorpt_correction_T_min  0.1139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       plate
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         10346
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0487P)^2^+13.5617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8106
_reflns_number_total             10346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj02982g2.cif
_cod_data_source_block           sun16
_cod_depositor_comments
'Adding full bibliography for 7060978--7060981.cif.'
_cod_database_code               7060978
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.454
_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.a Ternary CH refined with riding coordinates:
 C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C2(H2), C27(H27), C17(H17), C12(H12), C18(H18), C8(H8), C23(H23),
 C11(H11), C19(H19), C41(H41), C37(H37), C40(H40), C3(H3), C24(H24), C9(H9),
 C6(H6), C20(H20), C10(H10), C26(H26), C4(H4), C38(H38), C25(H25), C39(H39),
 C5(H5)
2.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C), C43(H43A,H43B,
 H43C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              96618
_olex2_submission_special_instructions 'No special instructions were received'