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_4349049
_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         'C108 H132 Ba2 Co4 N16 O24 S12, 2(C2 H3 N)'
_chemical_formula_sum            'C112 H138 Ba2 Co4 N18 O24 S12'
_chemical_formula_weight         3015.52
_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
_audit_creation_date             2015-10-29
_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                116.330(3)
_cell_angle_beta                 93.430(3)
_cell_angle_gamma                102.116(3)
_cell_formula_units_Z            1
_cell_length_a                   15.199(3)
_cell_length_b                   15.322(3)
_cell_length_c                   16.472(4)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.625
_cell_measurement_theta_min      2.331
_cell_volume                     3309.9(12)
_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 0.996
_diffrn_measured_fraction_theta_max 0.984
_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  0.0387
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            60531
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.783
_diffrn_reflns_theta_min         1.794
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.336
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0844 before and 0.0456 after correction.
The Ratio of minimum to maximum transmission is 0.8376.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       prism
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.27
_refine_diff_density_max         2.478
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     846
_refine_ls_number_reflns         20361
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+6.3182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16303
_reflns_number_total             20361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00233h2.cif
_cod_data_source_block           cmw-03-052
_cod_original_cell_volume        3309.8(12)
_cod_database_code               4349049
_olex2_refinement_description
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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
 S5-C39B \\sim S5-C39A
 with sigma of 0.002
3. Restrained planarity
 C39A, C40A, C41A, C42A, C43A, C44A, C45A
 with sigma of 0.002
 C39B, C40B, C41B, C42B, C43B, C44B
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
C39A \\sim C39B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C40A \\sim C40B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C41A \\sim C41B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C42A \\sim C42B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C45A \\sim C45B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C43A \\sim C43B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
C44A \\sim C44B: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
5. Rigid body (RIGU) restrains
 N9, C55, C57
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C28, C29, C30, C31, C32, C33, C34
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C39A, C40A, C41A, C42A, C43A, C44A, C45A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Same fragment restrains
{C39B, C40B, C41B, C42B, C43B, C44B, C45B} sigma for 1-2: 0.002, 1-3: 0.002
as
{C39A, C40A, C41A, C42A, C43A, C44A, C45A}
7. Others
 Sof(C39B)=Sof(C40B)=Sof(H40B)=Sof(C41B)=Sof(H41B)=Sof(C42B)=Sof(C43B)=
 Sof(H43B)=Sof(C44B)=Sof(H44B)=Sof(C45B)=Sof(H45D)=Sof(H45E)=Sof(H45F)=1-FVAR(1)
 Sof(C39A)=Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(C43A)=
 Sof(H43A)=Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(H45A)=Sof(H45B)=Sof(H45C)=FVAR(1)
8.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C12(H12A,H12B), C13(H13A,
 H13B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
 C46(H46A,H46B), C47(H47A,H47B)
8.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C10(H10), C15(H15), C16(H16), C18(H18), C19(H19),
 C22(H22), C23(H23), C25(H25), C26(H26), C29(H29), C30(H30), C32(H32), C33(H33),
  C49(H49), C50(H50), C52(H52), C53(H53), C40A(H40A), C41A(H41A), C43A(H43A),
 C44A(H44A), C40B(H40B), C41B(H41B), C43B(H43B), C44B(H44B)
8.c Idealised Me refined with riding coordinates:
 C45A(H45A,H45B,H45C)
8.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C34(H34A,H34B,
 H34C), C54(H54A,H54B,H54C), C45B(H45D,H45E,H45F), C57(H57A,H57B,H57C)
;
_shelx_res_checksum              4927
_shelx_hkl_checksum              54471
_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 CMW-03-052
_olex2_submission_special_instructions 'No special instructions were received'