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_7706926
_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         'C42 H76 Cr N2 Si2, C20 H40 K O8'
_chemical_formula_sum            'C62 H116 Cr K N2 O8 Si2'
_chemical_formula_weight         1164.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-22 deposited with the CCDC.	2021-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.2978(7)
_cell_length_b                   23.0874(9)
_cell_length_c                   34.2506(14)
_cell_measurement_reflns_used    13578
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.115
_cell_measurement_theta_min      2.128
_cell_volume                     13678.4(10)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_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 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_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  0.0914
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            239756
_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         26.115
_diffrn_reflns_theta_min         2.128
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1043 before and 0.0634 after correction. The Ratio of minimum to maximum transmission is 0.9241. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_description       block
_exptl_crystal_F_000             5096
_exptl_crystal_size_max          0.338
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         13578
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0296P)^2^+7.1646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0781
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10873
_reflns_number_total             13578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00121c2.cif
_cod_data_source_block           5_k_18c6_thf2_cr
_cod_depositor_comments
'Adding full bibliography for 7706910--7706927.cif.'
_cod_database_code               7706926
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.902
_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. Restrained distances
 C01D-C024 \\sim C01D-C0
 with sigma of 0.02
 C023-C024 \\sim C023-C0
 with sigma of 0.02
3. Others
 Fixed Sof: H0BA(0.5) HC(0.5) HD(0.5) HE(0.5) H02I(0.5) H02J(0.5) H02K(0.5)
 H02L(0.5) C024(0.666) H02M(0.666) H02N(0.666) C0(0.333) H0A(0.333) H0B(0.333)
4.a Ternary CH refined with riding coordinates:
 C00M(H00M), C00P(H00P), C00Q(H00Q), C00S(H00S), C00T(H00T), C00U(H00U),
 C00V(H00V), C00X(H00X), C00Z(H00Z), C012(H012)
4.b Secondary CH2 refined with riding coordinates:
 C010(H6AA,H), C015(H7AA,HA), C01A(H9AA,HB), C01D(H0BA,HC), C01D(HD,HE),
 C01E(H1BA,HF), C01F(H2BA,HG), C01K(H3BA,HN), C01M(H4BA,HQ), C01O(H5BA,HT),
 C01P(H6BA,HU), C01Q(H7BA,HV), C01S(H8BA,HY), C01T(H9BA,HZ), C01U(H0CA,H3CA),
 C01V(H1CA,H4CA), C01Z(H2CA,H1DA), C021(H02G,H02H), C023(H02I,H02J), C023(H02K,
 H02L), C024(H02M,H02N), C0(H0A,H0B)
4.c Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00N(H00N), C00O(H00O), C00W(H00W), C00Y(H00Y), C011(H011)
4.d Idealised Me refined as rotating group:
 C00R(H00A,H00B,H00C), C013(H01A,H01B,H01C), C014(H01D,H01E,H01F), C016(H01G,
 H01H,H01I), C017(H01J,H01K,H01L), C018(H01M,H01N,H01O), C01B(H01P,H01Q,H01R),
 C01C(H01S,H01T,H01U), C01G(H01V,H01W,H01X), C01H(H01Y,HH,HI), C01I(H01Z,HJ,HK),
  C01J(H01,HL,HM), C01L(H0AA,HO,HP), C01N(H1AA,HR,HS), C01R(H2AA,HW,HX),
 C01W(H3AA,H5CA,H6CA), C01X(H4AA,H7CA,H8CA), C01Y(H5AA,H9CA,H0DA), C020(H02A,
 H02B,H02C), C022(H02D,H02E,H02F)
;
_shelx_res_checksum              31131
_shelx_hkl_checksum              9958
_olex2_submission_special_instructions 'No special instructions were received'