Heterotrimetallic sandwich complexes supported by sulfonamido ligands
Wallen, Christian M.; Wielizcko, Marika; Bacsa, John; Scarborough, Christopher C.; Inorganic Chemistry Frontiers 3 (2016) 142–; doi:10.1039/C5QI00233H

data_4349057
_publ_section_title
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 Heterotrimetallic sandwich complexes supported by sulfonamido ligands
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              142
_journal_paper_doi               10.1039/C5QI00233H
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         'C43 H69 Co N5 O6 S3'
_chemical_formula_sum            'C43 H69 Co N5 O6 S3'
_chemical_formula_weight         907.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-25
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-10-30 deposited with the CCDC.
2015-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.4610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2734(9)
_cell_length_b                   14.8425(9)
_cell_length_c                   21.9158(14)
_cell_measurement_reflns_used    9735
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.551
_cell_measurement_theta_min      2.346
_cell_volume                     4533.6(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.11 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            104077
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.581
_diffrn_reflns_theta_min         1.562
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1158 before and 0.0616 after correction.
The Ratio of minimum to maximum transmission is 0.8727.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       prism
_exptl_crystal_F_000             1940
_exptl_crystal_size_max          0.428
_exptl_crystal_size_mid          0.427
_exptl_crystal_size_min          0.382
_refine_diff_density_max         1.983
_refine_diff_density_min         -1.670
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     762
_refine_ls_number_reflns         13895
_refine_ls_number_restraints     561
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0711
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+13.2629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1890
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10880
_reflns_number_total             13895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00233h2.cif
_cod_data_source_block           cmw04bucots
_cod_database_code               4349057
_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
 S1-C1B \\sim S1-C1A
 with sigma of 0.004
 C41B-C40 \\sim C41-C40
 with sigma of 0.005
 C20A-C19A \\sim C20B-C19B
 with sigma of 0.004
 C11B-C10B \\sim C9A-C8A \\sim C20B-C19B
 with sigma of 0.005
 N1-C8B \\sim N1-C8A
 with sigma of 0.005
 S3B-C21A \\sim S3B-C21B
 with sigma of 0.004
 S3B-N4B \\sim S3A-N4A
 with sigma of 0.02
 S3A-C21B \\sim S3B-C21A
 with sigma of 0.02
 N4A-C20A \\sim N4B-C20B
 with sigma of 0.004
3. Restrained planarity
 C1A, C2A, C3A, C4A, C5A, C6A, C7A
 with sigma of 0.004
 C1B, C2B, C3B, C4B, C5B, C6B, C7B
 with sigma of 0.004
 C21A, C22A, C23A, C24A, C25A, C26A, C27A
 with sigma of 0.004
 C21B, C22B, C23B, C24B, C25B, C26B, C27B
 with sigma of 0.004
4. Uiso/Uaniso restraints and constraints
C2A \\sim C2B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C3A \\sim C3B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C5A \\sim C5B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C6A \\sim C6B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C4A \\sim C4B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C7A \\sim C7B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C1A \\sim C1B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C20A \\sim C20B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C19A \\sim C19B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
N2A \\sim N2B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C10A \\sim C10B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.002
C11A \\sim C11B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C9A \\sim C9B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C8A \\sim C8B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
S3A \\sim S3B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
O5A \\sim O5B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
O6A \\sim O6B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
N4A \\sim N4B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.002
C21A \\sim C21B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C22A \\sim C22B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C23A \\sim C23B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C24A \\sim C24B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C25A \\sim C25B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C26A \\sim C26B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C27A \\sim C27B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C41B \\sim C41: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C42B \\sim C42: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C43 \\sim C43B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C19A \\sim C19B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
O5A \\sim O5B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
Uanis(C27A) \\sim Ueq, Uanis(C27B) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.004
Uanis(N4B) \\sim Ueq, Uanis(N4A) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
Uanis(S3A) \\sim Ueq, Uanis(S3B) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.002
Uanis(C41) \\sim Ueq, Uanis(C41B) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
Uanis(C8A) = Uanis(C8B)
Uanis(C9B) = Uanis(C9A)
Uanis(C20A) = Uanis(C20B)
Uanis(C27B) = Uanis(C27A)
5. Rigid body (RIGU) restrains
 N2A, C9A, C8A, N1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C19A, N2A, C9A, C10A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N1, C8B, C9B, N2B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C10B, C11B, N3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C19B, N2B, C9B, C10B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C21A, C22A, C23A, C24A, C25A, C26A, C27A, O6A, O5A, S3A, N4A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N4B, S3B, O5B, O6B, C21B, C22B, C23B, C24B, C25B, C26B, C27B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 N4A, C20A, C19A, N2A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C41, C42, C42B, C43, C41B, C43B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Same fragment restrains
{N4B, S3B, O5B, O6B, C21B, C22B, C23B, C24B, C25B, C26B, C27B} sigma for 1-2:
0.002, 1-3: 0.002
as
{N4A, S3A, O5A, O6A, C21A, C22A, C23A, C24A, C25A, C26A, C27A}
{N2B, C9B, C8B, C10B, C11B, C19B, C20B} sigma for 1-2: 0.002, 1-3: 0.002
as
{N2A, C9A, C8A, C10A, C11A, C19A, C20A}
{C1B, C2B, C3B, C4B, C5B, C6B, C7B} sigma for 1-2: 0.002, 1-3: 0.002
as
{C1A, C2A, C3A, C4A, C5A, C6A, C7A}
{C41B, C42B, C43B} sigma for 1-2: 0.002, 1-3: 0.002
as
{C41, C42, C43}
7. Others
 Sof(N4B)=Sof(S3B)=Sof(O5B)=Sof(O6B)=Sof(C21B)=Sof(C22B)=Sof(H22B)=Sof(C23B)=
 Sof(H23B)=Sof(C24B)=Sof(C25B)=Sof(H25B)=Sof(C26B)=Sof(H26B)=Sof(C27B)=
 Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(N2B)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(C8B)=
 Sof(H8BA)=Sof(H8BB)=Sof(C10B)=Sof(H10C)=Sof(H10D)=Sof(C11B)=Sof(H11C)=
 Sof(H11D)=Sof(C19B)=Sof(H19C)=Sof(H19D)=Sof(C20B)=Sof(H20C)=Sof(H20D)=Sof(C1B)=
 Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(C5B)=Sof(H5B)=Sof(C6B)=
 Sof(H6B)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(H7BC)=Sof(H40C)=Sof(H40D)=Sof(C41B)=
 Sof(H41C)=Sof(H41D)=Sof(C42B)=Sof(H42C)=Sof(H42D)=Sof(C43B)=Sof(H43D)=
 Sof(H43E)=Sof(H43F)=1-FVAR(1)
 Sof(N4A)=Sof(S3A)=Sof(O5A)=Sof(O6A)=Sof(C21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=
 Sof(H23A)=Sof(C24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=
 Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(N2A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C8A)=
 Sof(H8AA)=Sof(H8AB)=Sof(C10A)=Sof(H10A)=Sof(H10B)=Sof(C11A)=Sof(H11A)=
 Sof(H11B)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(C1A)=
 Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=
 Sof(H6A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(H40A)=Sof(H40B)=Sof(C41)=
 Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=
 Sof(H43C)=FVAR(1)
8.a Secondary CH2 refined with riding coordinates:
 C9A(H9AA,H9AB), C8A(H8AA,H8AB), C10A(H10A,H10B), C11A(H11A,H11B), C19A(H19A,
 H19B), C20A(H20A,H20B), C9B(H9BA,H9BB), C8B(H8BA,H8BB), C10B(H10C,H10D),
 C11B(H11C,H11D), C19B(H19C,H19D), C20B(H20C,H20D), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C32(H3,H2), C33(H33A,H33B), C34(H34A,H34B), C36(H4,H1),
 C37(H37A,H37B), C38(H38A,H38B), C40(H40A,H40B), C40(H40C,H40D), C41(H41A,H41B),
  C42(H42A,H42B), C41B(H41C,H41D), C42B(H42C,H42D)
8.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C16(H16), C17(H17), C22A(H22A), C23A(H23A), C25A(H25A),
 C26A(H26A), C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C22B(H22B), C23B(H23B),
 C25B(H25B), C26B(H26B), C2B(H2B), C3B(H3B), C5B(H5B), C6B(H6B)
8.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C27A(H27A,H27B,H27C), C7A(H7AA,H7AB,H7AC), C27B(H27D,
 H27E,H27F), C7B(H7BA,H7BB,H7BC), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C),
 C39(H39A,H39B,H39C), C43(H43A,H43B,H43C), C43B(H43D,H43E,H43F)
;
_shelx_res_checksum              52987
_shelx_hkl_checksum              40210
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id CMW04BuCoTs
_olex2_submission_special_instructions 'No special instructions were received'