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_7707907
_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         'C40 H56 Fe N2 Si2'
_chemical_formula_sum            'C40 H56 Fe N2 Si2'
_chemical_formula_weight         676.89
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-30
_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                117.2580(10)
_cell_angle_beta                 90.819(2)
_cell_angle_gamma                97.965(2)
_cell_formula_units_Z            4
_cell_length_a                   11.4603(5)
_cell_length_b                   19.4567(9)
_cell_length_c                   19.5695(9)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      2.24
_cell_volume                     3826.6(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      100.01
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            73224
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.289
_diffrn_reflns_theta_min         2.027
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.485
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0692 before and 0.0521 after correction. The Ratio of minimum to maximum transmission is 0.9603. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         17162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0254P)^2^+2.5563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12935
_reflns_number_total             17162
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01543e2.cif
_cod_data_source_block           fel1
_cod_depositor_comments
;
Adding full bibliography for 7707896--7707917.cif.

2025-01-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C80 H112 Fe2 N4 Si4'
_cod_original_formula_weight         1353.79
_cod_original_formula_moiety         '2(C40 H56 Fe N2 Si2)'
_cod_original_formula_units_Z            2
_cod_database_code               7707907
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.883
_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 Ternary CH refined with riding coordinates:
 C01C(H01I), C01F(H01), C01H(H1AA), C01M(H01M), C01N(H01N), C01Q(H5AA),
 C01U(H01U), C01X(H8AA)
2.b Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00J(H00J), C00M(H00M), C00R(H00R), C00U(H00U), C00W(H00W),
 C00Y(H00Y), C00Z(H00Z), C011(H011), C012(H012), C013(H013), C014(H014),
 C016(H016), C017(H017), C019(H019), C01A(H01G), C01B(H01H), C01D(H01J),
 C01E(H01Z), C01G(H0AA), C01I(H01K), C01J(H01L), C01K(H2AA), C01P(H4AA),
 C01R(H01R), C01T(H7AA), C01V(H01V), C01W(H01W), C01Y(H01Y), C020(H020),
 C022(H022), C024(H024)
2.c Idealised Me refined as rotating group:
 C00N(H00A,H00B,H00C), C010(H01A,H01B,H01C), C015(H01S,H01T,H01X), C018(H01D,
 H01E,H01F), C01L(H3AA,H,HA), C01O(H01O,H01P,H01Q), C01S(H6AA,HB,HC), C01Z(H9AA,
 HD,HE), C021(H02A,H02B,H02C), C023(H02Z,HF,HG), C025(H02D,H02E,H02F),
 C026(H02G,H02H,H02I), C027(H02J,H02K,H02L), C028(H02,HH,HI), C029(H02M,H02N,
 H02O), C02A(H0BA,HJ,HK), C02B(H02P,H02Q,H02R), C02C(H02S,H02T,H02U), C02D(H1BA,
 HL,HM), C02E(H2BA,HN,HO), C02F(H3BA,HP,HQ), C02G(H02V,H02W,H02X), C02H(H4BA,HR,
 HS), C02I(H02Y,HT,HU)
;
_shelx_res_checksum              21433
_shelx_hkl_checksum              77312
_olex2_submission_special_instructions 'No special instructions were received'