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_7706920
_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         'C78 H70 K2 Mn2 O2'
_chemical_formula_sum            'C78 H70 K2 Mn2 O2'
_chemical_formula_weight         1227.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 93.540(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6490(9)
_cell_length_b                   18.4355(9)
_cell_length_c                   19.6687(11)
_cell_measurement_reflns_used    7993
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.745
_cell_measurement_theta_min      2.31
_cell_volume                     6387.4(6)
_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_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0891
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37162
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.101
_diffrn_reflns_theta_max         25.101
_diffrn_reflns_theta_min         2.209
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1619 before and 0.0563 after correction. The Ratio of minimum to maximum transmission is 0.7512. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       needle
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.729
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     879
_refine_ls_number_reflns         11297
_refine_ls_number_restraints     1548
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.0829
_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^)+(0.0749P)^2^+21.3788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1868
_refine_ls_wR_factor_ref         0.2107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7145
_reflns_number_total             11297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00121c2.cif
_cod_data_source_block           13_k2_mn2_phccph_trimer
_cod_depositor_comments
'Adding full bibliography for 7706910--7706927.cif.'
_cod_database_code               7706920
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.680
_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
 C63-C77 \\sim C63-C71
 with sigma of 0.02
 C78-C79 \\sim C76-C75
 with sigma of 0.02
 C78-C77 \\sim C76-C71
 with sigma of 0.02
 C79-C80 \\sim C75-C74
 with sigma of 0.02
 C80-C81 \\sim C74-C73
 with sigma of 0.02
 C81-C82 \\sim C73-C72
 with sigma of 0.02
 C82-C77 \\sim C72-C71
 with sigma of 0.02
 C63-C78 \\sim C63-C76
 with sigma of 0.04
 C63-C82 \\sim C63-C72
 with sigma of 0.04
 C78-C80 \\sim C76-C74
 with sigma of 0.04
 C78-C82 \\sim C76-C72
 with sigma of 0.04
 C79-C81 \\sim C75-C73
 with sigma of 0.04
 C79-C77 \\sim C75-C71
 with sigma of 0.04
 C80-C82 \\sim C74-C72
 with sigma of 0.04
 C81-C77 \\sim C73-C71
 with sigma of 0.04
 C43-C57 \\sim C43-C51
 with sigma of 0.02
 C60-C59 \\sim C54-C53
 with sigma of 0.02
 C60-C61 \\sim C54-C55
 with sigma of 0.02
 C59-C58 \\sim C53-C52
 with sigma of 0.02
 C58-C57 \\sim C52-C51
 with sigma of 0.02
 C57-C62 \\sim C51-C56
 with sigma of 0.02
 C62-C61 \\sim C56-C55
 with sigma of 0.02
 C43-C58 \\sim C43-C52
 with sigma of 0.04
 C43-C62 \\sim C43-C56
 with sigma of 0.04
 C60-C58 \\sim C54-C52
 with sigma of 0.04
 C60-C62 \\sim C54-C56
 with sigma of 0.04
 C59-C57 \\sim C53-C51
 with sigma of 0.04
 C59-C61 \\sim C53-C55
 with sigma of 0.04
 C58-C62 \\sim C52-C56
 with sigma of 0.04
 C57-C61 \\sim C51-C55
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C3AA) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C55) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C53) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C78) = Uanis(C81)
Uanis(C8AA) = Uanis(C0BA)
Uanis(C9AA) = Uanis(C7AA)
Uanis(C5BA) = Uanis(C8AA) = Uanis(C0BA)
Uanis(C4BA) = Uanis(C3BA) = Uanis(C0AA) = Uanis(C2BA)
Uanis(C6AA) = Uanis(C2AA) = Uanis(C1AA) = Uanis(C5AA)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C60(0.5) H60(0.5) C59(0.5) H59(0.5) C58(0.5) H58(0.5) C57(0.5)
 C62(0.5) H62(0.5) C61(0.5) H61(0.5) C78(0.5) H78(0.5) C79(0.5) H79(0.5)
 C80(0.5) H80(0.5) C81(0.5) H81(0.5) C82(0.5) H82(0.5) C77(0.5) C51(0.5)
 C52(0.5) H52(0.5) C53(0.5) H53(0.5) C54(0.5) H54(0.5) C55(0.5) H55(0.5)
 C56(0.5) H56(0.5) C71(0.5) C72(0.5) H72(0.5) C73(0.5) H73(0.5) C74(0.5)
 H74(0.5) C75(0.5) H75(0.5) C76(0.5) H76(0.5) O1(0.5) O4(0.5) O6(0.5) C1AA(0.5)
 H1AA(0.5) H1AB(0.5) C2AA(0.5) H2AA(0.5) H2AB(0.5) C5AA(0.5) H5AA(0.5)
 H5AB(0.5) H5AC(0.5) C6AA(0.5) H6AA(0.5) H6AB(0.5) H6AC(0.5) C3AA(0.5)
 H3AA(0.5) H3AB(0.5) H3AC(0.5) C7AA(0.5) H7AA(0.5) H7AB(0.5) C8AA(0.5)
 H8AA(0.5) H8AB(0.5) C9AA(0.5) H9AA(0.5) H9AB(0.5) C0BA(0.5) H0BA(0.5)
 H0BB(0.5) O2(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5) C2BA(0.5) H2BA(0.5) H2BB(0.5)
 H2BC(0.5) C3BA(0.5) H3BA(0.5) H3BB(0.5) C4BA(0.5) H4BA(0.5) H4BB(0.5)
 H4BC(0.5) C4AA(0.5) H4AA(0.5) H4AB(0.5) H4AC(0.5) C5BA(0.5) H5BA(0.5)
 H5BB(0.5) H5BC(0.5) C1BA(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB), C2AA(H2AA,H2AB), C7AA(H7AA,H7AB), C8AA(H8AA,H8AB), C9AA(H9AA,
 H9AB), C0BA(H0BA,H0BB), C0AA(H0AA,H0AB), C3BA(H3BA,H3BB)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C46(H46),
  C47(H47), C48(H48), C49(H49), C50(H50), C66(H66), C67(H67), C68(H68),
 C69(H69), C70(H70), C60(H60), C59(H59), C58(H58), C62(H62), C61(H61), C78(H78),
  C79(H79), C80(H80), C81(H81), C82(H82), C52(H52), C53(H53), C54(H54),
 C55(H55), C56(H56), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76)
6.c Fitted hexagon refined as free rotating group:
 C60(C59,C58,C57,C62,C61), C78(C79,C80,C81,C82,C77)
6.d Idealised Me refined as rotating group:
 C5AA(H5AA,H5AB,H5AC), C6AA(H6AA,H6AB,H6AC), C3AA(H3AA,H3AB,H3AC), C2BA(H2BA,
 H2BB,H2BC), C4BA(H4BA,H4BB,H4BC), C4AA(H4AA,H4AB,H4AC), C5BA(H5BA,H5BB,H5BC),
 C1BA(H1BA,H1BB,H1BC)
;
_shelx_res_checksum              57826
_shelx_hkl_checksum              39181
_olex2_submission_special_instructions 'No special instructions were received'