Homoleptic quasilinear metal(i/ii) silylamides of Cr-Co with phenyl and allyl functions - impact of the oxidation state on secondary ligand interactions.
Weller, Ruth; Ruppach, Lutz; Shlyaykher, Alena; Tambornino, Frank; Werncke, C. Gunnar; Dalton transactions (Cambridge, England : 2003) 50 (2021) 10947–10963; doi:10.1039/d1dt01543e

data_7707898
_publ_section_title
;
 Homoleptic quasilinear metal(i/ii) silylamides of Cr-Co with phenyl and
 allyl functions - impact of the oxidation state on secondary ligand
 interactions.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10947
_journal_page_last               10963
_journal_paper_doi               10.1039/d1dt01543e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C46 H80 Co K N2 O6 Si2'
_chemical_formula_sum            'C46 H80 Co K N2 O6 Si2'
_chemical_formula_weight         911.33
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-12 deposited with the CCDC.	2021-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.376(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0369(5)
_cell_length_b                   22.1041(11)
_cell_length_c                   18.2404(7)
_cell_measurement_reflns_used    10419
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.748
_cell_measurement_theta_min      2.485
_cell_volume                     4927.4(4)
_computing_cell_refinement       'X-Area Recipe 1.36.0.0 (STOE, 2020)'
_computing_data_collection       'X-Area WinXpose 2.0.22.0 (STOE, 2016)'
_computing_data_reduction        'X-Area X-Red 1.65.2.0 (STOE, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'imaging plate area detector'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5 mm, multiple pinhole'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39565
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.748
_diffrn_reflns_theta_min         2.485
_diffrn_source                   'sealed X-ray tube, 12 x 0.4 mm LF focus'
_diffrn_source_target            Mo
_diffrn_source_type              'STOE C-Tech Mo LFF X-Ray Tube'
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.9512
_exptl_absorpt_correction_T_min  0.6344
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
X-Area LANA 1.71.6.0 (STOE, 2017) Statistics over combined scale factors for x file reflections:
       min. = 0.745 (run 1)   max. = 1.118 (run 1)    spread = 0.4
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       plate
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.415
_exptl_crystal_size_mid          0.395
_exptl_crystal_size_min          0.101
_exptl_crystal_size_rad          0.062
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         10419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0365P)^2^+1.4049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7952
_reflns_number_total             10419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01543e2.cif
_cod_data_source_block           k18c6_col4
_cod_depositor_comments
'Adding full bibliography for 7707896--7707917.cif.'
_cod_database_code               7707898
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.811
_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:
 C00F(H00F), C00I(H00I), C00J(H00J), C00N(H00N)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C014(H01G,H01H), C015(H01I,H01J), C016(H01K,H01L), C018(H01P,
 H01Q), C01B(H01X,H01Y), C01C(H01Z,H), C01E(H1,HC), C01F(H3,HD), C01G(H4,HE),
 C01H(H6,HF), C01L(H10,HM), C01M(H11,HN)
2.c Aromatic/amide H refined with riding coordinates:
 C00S(H00S), C00U(H00U), C00V(H00V), C00Y(H00Y), C010(H010), C012(H012)
2.d Idealised Me refined as rotating group:
 C00T(H00A,H00B,H00C), C00W(H00D,H00E,H00G), C00Z(H00H,H00K,H00L), C017(H01M,
 H01N,H01O), C019(H01R,H01S,H01T), C01A(H01U,H01V,H01W), C01D(H01,HA,HB),
 C01I(H7,HG,HH), C01J(H8,HI,HJ), C01K(H9,HK,HL)
;
_shelx_res_checksum              84761
_shelx_hkl_checksum              70581
_olex2_submission_special_instructions 'No special instructions were received'