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_4349058
_publ_section_title
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 Heterotrimetallic sandwich complexes supported by sulfonamido ligands
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_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
'C27 H35 Co N4 O7 S3 Sr2, C27 H35 Co N4 O7 S3, 2(C27 H33 Co N4 O6 S3), O'
_chemical_formula_sum            'C108 H138 Co4 N16 O27 S12 Sr2'
_chemical_formula_weight         2888.02
_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   mixed
_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                90
_cell_angle_beta                 95.585(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.583(7)
_cell_length_b                   16.185(4)
_cell_length_c                   25.822(6)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.541
_cell_measurement_theta_min      2.188
_cell_volume                     12305(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.1-1 (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 1.000
_diffrn_measured_fraction_theta_max 0.936
_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  0.0842
_diffrn_reflns_av_unetI/netI     0.1103
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            97100
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.603
_diffrn_reflns_theta_min         0.692
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.669
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.3494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1695 before and 0.0606 after correction.
The Ratio of minimum to maximum transmission is 0.4684.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       plate
_exptl_crystal_F_000             5960
_exptl_crystal_size_max          0.915
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.096
_refine_diff_density_max         1.516
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1537
_refine_ls_number_reflns         32412
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.0630
_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^)+(0.0666P)^2^+1.4189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20137
_reflns_number_total             32412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00233h2.cif
_cod_data_source_block           cmw-03-086srts
_cod_database_code               4349058
_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, All Sr(H,H,H,H) groups
2. Restrained distances
 O1-H1A = O1-H1B
 0.975 with sigma of 0.005
 H1A-H1B
 1.555 with sigma of 0.01
 H1A-O4
 1.695 with sigma of 0.02
 H1B-O24
 1.795 with sigma of 0.02
 O19_$1-H8D
 1.695 with sigma of 0.02
 O8-H8C = O8-H8D
 0.975 with sigma of 0.005
 H8D-H8C
 1.555 with sigma of 0.01
 O10-H8C
 1.555 with sigma of 0.01
3. Others
 Fixed X: H1A(0.284709) H1B(0.239969) H8C(0.26842)
 Fixed Y: H1A(0.16709) H1B(0.167681) H8C(0.6723)
 Fixed Z: H1A(0.255529) H1B(0.21885) H8C(0.2842)
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C20(H20A,H20B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C19(H19A,H19B), C47(H47A,H47B), C36(H36A,H36B), C35(H35A,H35B), C38(H38A,H38B),
  C37(H37A,H37B), C46(H46A,H46B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,
 H64B), C65(H65A,H65B), C74(H74A,H74B), C73(H73A,H73B), C89(H89A,H89B),
 C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B), C101(H10C,H10D), C100(H10E,
 H10F)
4.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C2(H2), C14(H14), C3(H3), C13(H13), C16(H16), C26(H26),
 C17(H17), C6(H6), C5(H5), C25(H25), C43(H43), C41(H41), C29(H29), C50(H50),
 C49(H49), C53(H53), C40(H40), C30(H30), C44(H44), C32(H32), C33(H33), C52(H52),
  C77(H77), C76(H76), C56(H56), C57(H57), C59(H59), C60(H60), C80(H80),
 C79(H79), C67(H67), C68(H68), C70(H70), C71(H71), C83(H83), C84(H84), C86(H86),
  C87(H87), C103(H103), C104(H104), C106(H106), C107(H107), C94(H94), C95(H95),
 C97(H97), C98(H98)
4.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C7(H7A,H7B,H7C), C27(H27A,H27B,H27C), C54(H54A,H54B,
 H54C), C34(H34A,H34B,H34C), C45(H45A,H45B,H45C), C61(H61A,H61B,H61C), C81(H81A,
 H81B,H81C), C72(H72A,H72B,H72C), C88(H88A,H88B,H88C), C108(H10G,H10H,H10I),
 C99(H99A,H99B,H99C)
;
_shelx_res_checksum              9248
_shelx_hkl_checksum              679
_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-030086SRTS
_olex2_submission_special_instructions 'No special instructions were received'