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_4349053
_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 Ca1 Co2 N8 O12 S6'
_chemical_formula_sum            'C36 H78 Ca Co2 N8 O12 S6'
_chemical_formula_weight         1165.36
_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   mixed
_audit_creation_date             2015-10-28
_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                   12.601(3)
_cell_length_b                   12.601(3)
_cell_length_c                   29.273(8)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.920
_cell_measurement_theta_min      2.328
_cell_volume                     4025.4(17)
_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 0.997
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans with a narrow frame width'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            17386
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.068
_diffrn_reflns_theta_min         2.087
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.4389
_exptl_absorpt_correction_T_min  0.3299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0977 before and 0.0604 after correction.
The Ratio of minimum to maximum transmission is 0.7517.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       prism
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.906
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         4461
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0595P)^2^+1.4018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3518
_reflns_number_total             4461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00233h2.cif
_cod_data_source_block           cmw_03_020
_cod_original_cell_volume        4025(2)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4349053
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.683
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, {H5B,H5A} of C5
 At 1.2 times of:
  {H1A,H1B} of C1, {H2BA,H2BB} of C2B, {H1BA,H1BB} of C1B, {H2B,H2A} of C2
2. Restrained distances
 N1-C1 \\sim N1-C1B
 with sigma of 0.002
 C2B-C1B \\sim C2-C1
 with sigma of 0.002
 N2-C2 \\sim N2-C2B
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
C1 \\sim C1B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C2B \\sim C2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C1B) = Uanis(C1)
Uanis(C2B) = Uanis(C2)
4. Rigid body (RIGU) restrains
 N2, C2B, C2, C1, C1B, N1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2B)=Sof(H2A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2B,H2A), C1B(H1BA,H1BB), C2B(H2BA,H2BB)
6.b Idealised Me refined as rotating group:
 C4(H4A,H4C,H4B), C6(H6B,H6A,H6C)
;
_shelx_res_checksum              1448
_shelx_hkl_checksum              65238
_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-03-020
_olex2_submission_special_instructions 'No special instructions were received'