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_4349051
_publ_section_title
;
 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         'C18 H39 Co N4 O6 S3, C14 H36 N1'
_chemical_formula_sum            'C34 H75 Co N5 O6 S3'
_chemical_formula_weight         805.10
_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
_audit_creation_date             2015-10-30
_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                 99.185(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.505(2)
_cell_length_b                   11.3473(14)
_cell_length_c                   19.833(2)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.175
_cell_measurement_theta_min      2.403
_cell_volume                     4333.3(8)
_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 0.995
_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  0.0614
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            51543
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.199
_diffrn_reflns_theta_min         2.074
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0821 before and 0.0579 after correction.
The Ratio of minimum to maximum transmission is 0.8248.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       prism
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.478
_exptl_crystal_size_min          0.236
_refine_diff_density_max         1.584
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     848
_refine_ls_number_reflns         11684
_refine_ls_number_restraints     1142
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1176
_refine_ls_R_factor_gt           0.0835
_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^)+(0.0797P)^2^+17.4306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1963
_refine_ls_wR_factor_ref         0.2199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8299
_reflns_number_total             11684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00233h2.cif
_cod_data_source_block           cmw04bucobus
_cod_original_cell_volume        4333.3(9)
_cod_database_code               4349051
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.732
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C21A-C20A = C29A-C28A = C33A-C32A = C25A-C24A
 1.525 with sigma of 0.005
 C34A-C33A \\sim C26A-C25A \\sim C30A-C29A \\sim C22A-C21A
 with sigma of 0.005
 C25A-C24A \\sim C33A-C32A \\sim C29A-C28A \\sim C21A-C20A
 with sigma of 0.005
 C34A-C32A \\sim C22A-C20A \\sim C26A-C24A \\sim C30A-C28A
 with sigma of 0.005
 C22B-C20B \\sim C30B-C28B \\sim C26B-C24B \\sim C34B-C32B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
N5B \\sim N5A: 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
C23B \\sim C23A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C27B \\sim C27A: 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
C24A \\sim C24B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C32A \\sim C32B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C28A \\sim C28B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C21B \\sim C21A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C25B \\sim C25A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C33B \\sim C33A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C29B \\sim C29A: 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
C26A \\sim C26B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C34B \\sim C34A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C30A \\sim C30B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C31B \\sim C31A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
N4B \\sim N4A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
S1B \\sim S1A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
O1B \\sim O1A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
O2B \\sim O2A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C7B \\sim C7A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C6B \\sim C6A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C8B \\sim C8A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C9B \\sim C9A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C10B \\sim C10A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C5B \\sim C5A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
N2B \\sim N2A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C2B \\sim C2A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C3B \\sim C3A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C1B \\sim C1A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C4B \\sim C4A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
N1B \\sim N1A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
N3B \\sim N3A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
S3B \\sim S3A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
S2B \\sim S2A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
O5B \\sim O5A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
O6B \\sim O6A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C15B \\sim C15A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
O3B \\sim O3A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
O4B \\sim O4A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C11B \\sim C11A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C16B \\sim C16A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C17B \\sim C17A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C18B \\sim C18A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C12B \\sim C12A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C13B \\sim C13A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
C14A \\sim C14B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(S3A) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(N2A) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(N3B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(N1A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(S3B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O5A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C5B) = Uanis(C5A)
Uanis(N2B) = Uanis(N2A)
Uanis(N1A) = Uanis(N1B)
Uanis(N4A) = Uanis(N4B)
Uanis(N3A) = Uanis(N3B)
Uanis(O3B) = Uanis(O3A)
Uanis(O4A) = Uanis(O4B)
Uanis(S2B) = Uanis(S2A)
Uanis(C7B) = Uanis(C7A)
4. Rigid body (RIGU) restrains
 C21A, C19A, C20A, C23A, C24A, C25A, C22A, C26A, C28A, C29A, C30A, C31A, C32A,
 C33A, C34A, C27A, N5A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C25B, C21B, C29B, C33B, C23B, C27B, C31B, C20B, N5B, C22B, C24B, C26B, C28B,
 C30B, C32B, C34B, C19B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A, C11A, C12A, C13A, C14A,
 C15A, C16A, C17A, C18A, N1A, N2A, N3A, N4A, O1A, O2A, O3A, O4A, O5A, O6A, S1A,
 S2A, S3A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, C10B, C11B, C12B, C13B, C14B,
 C15B, C16B, C17B, C18B, N1B, N2B, N3B, N4B, O1B, O2B, O3B, O4B, O5B, O6B, S1B,
 S2B, S3B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Same fragment restrains
{C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A, C11A, C12A, C13A, C14A,
C15A, C16A, C17A, C18A, N1A, N2A, N3A, N4A, O1A, O2A, O3A, O4A, O5A, O6A, S1A,
S2A, S3A} sigma for 1-2: 0.002, 1-3: 0.004
as
{C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, C10B, C11B, C12B, C13B, C14B,
C15B, C16B, C17B, C18B, N1B, N2B, N3B, N4B, O1B, O2B, O3B, O4B, O5B, O6B, S1B,
S2B, S3B}
{C25A, C21A, C29A, C33A, C23A, C27A, C31A, C20A, N5A, C22A, C24A, C26A, C28A,
C30A, C32A, C34A, C19A} sigma for 1-2: 0.002, 1-3: 0.004
as
{C25B, C21B, C29B, C33B, C23B, C27B, C31B, C20B, N5B, C22B, C24B, C26B, C28B,
C30B, C32B, C34B, C19B}
6. Others
 Sof(C25B)=Sof(H25A)=Sof(H25B)=Sof(C21B)=Sof(H21A)=Sof(H21B)=Sof(C29B)=
 Sof(H29A)=Sof(H29B)=Sof(C23B)=Sof(H23A)=Sof(H23B)=Sof(C27B)=Sof(H27A)=
 Sof(H27B)=Sof(C31B)=Sof(H31A)=Sof(H31B)=Sof(C20B)=Sof(H20A)=Sof(H20B)=Sof(N5B)=
 Sof(C22B)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C24B)=Sof(H24A)=Sof(H24B)=
 Sof(C26B)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C28B)=Sof(H28A)=Sof(H28B)=
 Sof(C30B)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C32B)=Sof(H32A)=Sof(H32B)=
 Sof(C34B)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C19B)=Sof(H19A)=Sof(H19B)=
 Sof(C33A)=Sof(H33C)=Sof(H33D)=1-FVAR(1)
 Sof(C33B)=Sof(H33A)=Sof(H33B)=Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C21A)=
 Sof(H21C)=Sof(H21D)=Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C23A)=Sof(H23C)=
 Sof(H23D)=Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C31A)=Sof(H31C)=Sof(H31D)=
 Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(N5A)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=
 Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=
 Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=
 Sof(C32A)=Sof(H32C)=Sof(H32D)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=
 Sof(C19A)=Sof(H19C)=Sof(H19D)=FVAR(1)
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=
 Sof(H3BB)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C6B)=
 Sof(H6BA)=Sof(H6BB)=Sof(C7B)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=Sof(C9B)=
 Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C10B)=Sof(H10A)=Sof(H10B)=Sof(H10C)=
 Sof(C11B)=Sof(C12B)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13B)=Sof(H13A)=
 Sof(H13B)=Sof(H13C)=Sof(C14B)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15B)=
 Sof(C16B)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17B)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=Sof(C18B)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(N1B)=Sof(N2B)=Sof(N3B)=
 Sof(N4B)=Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=Sof(S1B)=
 Sof(S2B)=Sof(S3B)=1-FVAR(2)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=
 Sof(H6AA)=Sof(H6AB)=Sof(C7A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=
 Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=
 Sof(C11A)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C13A)=Sof(H13D)=
 Sof(H13E)=Sof(H13F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15A)=
 Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=
 Sof(H17F)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(N1A)=Sof(N2A)=Sof(N3A)=
 Sof(N4A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(S1A)=
 Sof(S2A)=Sof(S3A)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C1B(H1BA,H1BB), C2B(H2BA,H2BB), C3B(H3BA,H3BB), C4B(H4BA,H4BB), C5B(H5BA,
 H5BB), C6B(H6BA,H6BB), C1A(H1AA,H1AB), C2A(H2AA,H2AB), C3A(H3AA,H3AB),
 C4A(H4AA,H4AB), C5A(H5AA,H5AB), C6A(H6AA,H6AB), C25B(H25A,H25B), C21B(H21A,
 H21B), C29B(H29A,H29B), C33B(H33A,H33B), C23B(H23A,H23B), C27B(H27A,H27B),
 C31B(H31A,H31B), C20B(H20A,H20B), C24B(H24A,H24B), C28B(H28A,H28B), C32B(H32A,
 H32B), C19B(H19A,H19B), C25A(H25C,H25D), C21A(H21C,H21D), C29A(H29C,H29D),
 C33A(H33C,H33D), C23A(H23C,H23D), C27A(H27C,H27D), C31A(H31C,H31D), C20A(H20C,
 H20D), C24A(H24C,H24D), C28A(H28C,H28D), C32A(H32C,H32D), C19A(H19C,H19D)
7.b Idealised Me refined as rotating group:
 C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C10B(H10A,H10B,H10C), C12B(H12A,
 H12B,H12C), C13B(H13A,H13B,H13C), C14B(H14A,H14B,H14C), C16B(H16A,H16B,H16C),
 C17B(H17A,H17B,H17C), C18B(H18A,H18B,H18C), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,
 H9AC), C10A(H10D,H10E,H10F), C12A(H12D,H12E,H12F), C13A(H13D,H13E,H13F),
 C14A(H14D,H14E,H14F), C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F), C18A(H18D,
 H18E,H18F), C22B(H22A,H22B,H22C), C26B(H26A,H26B,H26C), C30B(H30A,H30B,H30C),
 C34B(H34A,H34B,H34C), C22A(H22D,H22E,H22F), C26A(H26D,H26E,H26F), C30A(H30D,
 H30E,H30F), C34A(H34D,H34E,H34F)
;
_shelx_res_checksum              87361
_shelx_hkl_checksum              18277
_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 CMW04BuCoBus
_olex2_submission_special_instructions 'No special instructions were received'