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_4349056
_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         'C36 H78 Co2 N8 O12 S6 Sr1'
_chemical_formula_sum            'C36 H78 Co2 N8 O12 S6 Sr'
_chemical_formula_weight         1212.90
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   12.638(4)
_cell_length_b                   12.638(4)
_cell_length_c                   29.797(8)
_cell_measurement_reflns_used    5438
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.492
_cell_measurement_theta_min      3.224
_cell_volume                     4122(2)
_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 0.998
_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  0.0343
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            16290
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.513
_diffrn_reflns_theta_min         1.982
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.850
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0685 before and 0.0489 after correction.
The Ratio of minimum to maximum transmission is 0.7793.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       prism
_exptl_crystal_F_000             1902
_exptl_crystal_size_max          0.363
_exptl_crystal_size_mid          0.287
_exptl_crystal_size_min          0.196
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2798
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+3.6001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2518
_reflns_number_total             2798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00233h2.cif
_cod_data_source_block           CoSrCoBus
_cod_original_cell_volume        4122(3)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4349056
_shelx_estimated_absorpt_t_max   0.713
_shelx_estimated_absorpt_t_min   0.553
_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. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C2)
Uanis(N2) = Uanis(N2')
3. Same fragment restrains
{C1', C2', N2'} sigma for 1-2: 0.002, 1-3: 0.002
as
{C1, C2, N2}
4. Others
 Sof(C1')=Sof(H1'A)=Sof(H1'B)=Sof(C2')=Sof(H2'B)=Sof(H2'A)=Sof(N2')=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(N2)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C1'(H1'A,H1'B), C2'(H2'B,H2'A)
5.b Idealised Me refined as rotating group:
 C4(H4A,H4C,H4B), C5(H5A,H5C,H5B), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              87995
_shelx_hkl_checksum              10838
_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-03-050
_olex2_submission_special_instructions 'No special instructions were received'