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_7707903
_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         'C52 H73 Co N3 Si2, C20 H40 K O8'
_chemical_formula_sum            'C72 H113 Co K N3 O8 Si2'
_chemical_formula_weight         1302.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-12 deposited with the CCDC.	2021-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.265(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1708(6)
_cell_length_b                   25.7371(18)
_cell_length_c                   28.1136(15)
_cell_measurement_reflns_used    7779
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.754
_cell_measurement_theta_min      2.59
_cell_volume                     7359.1(8)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (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 0.998
_diffrn_measured_fraction_theta_max 0.992
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            31700
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.754
_diffrn_reflns_theta_min         2.590
_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    0.375
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.7714
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
X-Area LANA 1.83.8.0 (STOE, 2020)   Statistics over combined scale factors for x file reflections:
       min. = 0.867 (run 2)   max. = 1.123 (run 1)    spread = 0.3
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       block
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.501
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.152
_exptl_crystal_size_rad          0.062
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0461P)^2^+3.6701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6194
_reflns_number_total             7779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01543e2.cif
_cod_data_source_block           k18c6_col1_ndipp
_cod_depositor_comments
'Adding full bibliography for 7707896--7707917.cif.'
_cod_database_code               7707903
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.834
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H01J(0.75) H01K(0.75) H01L(0.25) H01M(0.25) H01N(0.75) H01O(0.75)
 H01P(0.25) H01Q(0.25) C019(0.75) H01R(0.75) H01S(0.75) C01A(0.75) H01T(0.75)
 H01U(0.75) C0AA(0.25) H0AB(0.25) H0AC(0.25) C1AA(0.25) H1AB(0.25) H1AC(0.25)
3.a Ternary CH refined with riding coordinates:
 C00H(H00H), C00L(H00L), C00P(H00P)
3.b Secondary CH2 refined with riding coordinates:
 C00J(H00X,H00Y), C00M(H00,H), C00N(H0AA,HA), C00Q(H1AA,HB), C00S(H2AA,HC),
 C00U(H3AA,HD), C017(H01J,H01K), C017(H01L,H01M), C018(H01N,H01O), C018(H01P,
 H01Q), C019(H01R,H01S), C01A(H01T,H01U), C0AA(H0AB,H0AC), C1AA(H1AB,H1AC)
3.c Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00O(H00O), C00R(H00R), C00T(H00T), C00W(H00W), C00Z(H00Z),
 C011(H011), C012(H012), C013(H013), C016(H016)
3.d Idealised Me refined as rotating group:
 C00C(H00A,H00B,H00C), C00I(H00D,H00E,H00F), C00V(H00I,H00J,H00K), C00X(H00M,
 H00N,H00Q), C00Y(H00S,H00U,H00V), C010(H01A,H01B,H01C), C014(H01D,H01E,H01F),
 C015(H01G,H01H,H01I)
;
_shelx_res_checksum              20239
_shelx_hkl_checksum              91769
_olex2_submission_special_instructions 'No special instructions were received'