Quasilinear 3d-metal(i) complexes [KM(N(Dipp)SiR<sub>3</sub>)<sub>2</sub>] (M = Cr-Co) - structural diversity, solution state behaviour and reactivity.
Weller, Ruth; Müller, Igor; Duhayon, Carine; Sabo-Etienne, Sylviane; Bontemps, Sébastien; Werncke, C. Gunnar; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4890–4903; doi:10.1039/d1dt00121c

data_7706915
_publ_section_title
;
 Quasilinear 3d-metal(i) complexes
 [KM(N(Dipp)SiR<sub>3</sub>)<sub>2</sub>] (M = Cr-Co) - structural
 diversity, solution state behaviour and reactivity.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4890
_journal_page_last               4903
_journal_paper_doi               10.1039/d1dt00121c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C37 H60 Co K N2 Si2'
_chemical_formula_sum            'C37 H60 Co K N2 Si2'
_chemical_formula_weight         687.08
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-18 deposited with the CCDC.	2021-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 128.3810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.6815(11)
_cell_length_b                   25.6246(11)
_cell_length_c                   15.9053(7)
_cell_measurement_reflns_used    9216
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.052
_cell_measurement_theta_min      2.558
_cell_volume                     7885.5(6)
_computing_cell_refinement       '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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_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 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            141451
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.106
_diffrn_reflns_theta_min         2.279
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1310 before and 0.0587 after correction. The Ratio of minimum to maximum transmission is 0.9257. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       needle
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.567
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.143
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         7826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0129P)^2^+19.4738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6748
_reflns_number_total             7826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00121c2.cif
_cod_data_source_block           4_kco
_cod_depositor_comments
'Adding full bibliography for 7706910--7706927.cif.'
_cod_database_code               7706915
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.717
_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:
 C00F(H00F), C00H(H00H), C00I(H00I), C00N(H00N)
2.b Aromatic/amide H refined with riding coordinates:
 C008(H008), C00D(H00D), C00E(H00E), C00G(H00G), C00M(H00M), C00O(H00O),
 C00U(H00Z), C00W(H0AA), C010(H010), C011(H011), C012(H012)
2.c Idealised Me refined as rotating group:
 C00P(H00J,H00K,H00L), C00Q(H00P,H00Q,H00R), C00R(H00S,H00T,H00U), C00S(H00V,
 H00W,H00X), C00T(H00Y,H,HA), C00V(H00,HB,HC), C00X(H1AA,HD,HE), C00Y(H2AA,HF,
 HG), C00Z(H3AA,HH,HI), C013(H01A,H01B,H01C), C014(H01D,H01E,H01F), C015(H01G,
 H01H,H01I), C016(H01J,H01K,H01L), C017(H01M,H01N,H01O)
;
_shelx_res_checksum              86210
_shelx_hkl_checksum              93550
_olex2_submission_special_instructions 'No special instructions were received'