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_7706921
_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         'C74 H103 K2 Mn2 N2 O4 Si2'
_chemical_formula_sum            'C74 H103 K2 Mn2 N2 O4 Si2'
_chemical_formula_weight         1328.84
_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             2021-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-24 deposited with the CCDC.	2021-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                104.35(5)
_cell_angle_beta                 107.84(6)
_cell_angle_gamma                105.11(6)
_cell_formula_units_Z            1
_cell_length_a                   12.905(11)
_cell_length_b                   13.215(8)
_cell_length_c                   14.360(9)
_cell_measurement_reflns_used    2800
_cell_measurement_temperature    100
_cell_measurement_theta_max      17.86
_cell_measurement_theta_min      1.57
_cell_volume                     2103(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_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  0.1069
_diffrn_reflns_av_unetI/netI     0.0991
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15985
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.594
_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    0.468
_exptl_absorpt_correction_T_max  0.9199
_exptl_absorpt_correction_T_min  0.4475
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Area X-Red 1.63.1.0 (STOE, 2016)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_description       plate
_exptl_crystal_F_000             709
_exptl_crystal_size_max          0.942
_exptl_crystal_size_mid          0.456
_exptl_crystal_size_min          0.229
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         7390
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0868
_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^)+(0.1644P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2314
_refine_ls_wR_factor_ref         0.2483
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4387
_reflns_number_total             7390
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00121c2.cif
_cod_data_source_block           12_k2_mn2_phccph2
_cod_depositor_comments
'Adding full bibliography for 7706910--7706927.cif.'
_cod_database_code               7706921
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.667
_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. Restrained distances
 C38-C37
 1.5 with sigma of 0.02
 C24-C27 \\sim C24-C26
 with sigma of 0.02
 Si1-C30 \\sim Si1-C31
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C31) = Uanis(C30)
4. Others
 Fixed Sof: H24(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5) C30(0.5) H30A(0.5)
 H30B(0.5) H30C(0.5) C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C31(0.5) H31A(0.5)
 H31B(0.5) H31C(0.5)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C21(H21), C24(H24)
5.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,
 H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C17(H17), C18(H18), C19(H19)
5.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C26(H26A,
 H26B,H26C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              95179
_shelx_hkl_checksum              2001
_shelx_fab_checksum              55893
_olex2_submission_special_instructions 'No special instructions were received'