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_4349054
_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_absolute_configuration unk
_chemical_formula_moiety         'C54 H66 Ca Co2 N8 O12 S6'
_chemical_formula_sum            'C54 H66 Ca Co2 N8 O12 S6'
_chemical_formula_weight         1369.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                 112.3550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9236(11)
_cell_length_b                   13.3642(10)
_cell_length_c                   17.2950(13)
_cell_measurement_reflns_used    7388
_cell_measurement_temperature    109.01
_cell_measurement_theta_max      29.09
_cell_measurement_theta_min      2.20
_cell_volume                     2976.4(4)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'APEX2 v2011.2-4 (Bruker, 2011)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      109.01
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 1.000
_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  0.0328
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22136
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.216
_diffrn_reflns_theta_min         1.581
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0641 before and 0.0505 after correction.
The Ratio of minimum to maximum transmission is 0.7802.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear bluish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.063
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.194(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         14778
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0624P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1128
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                13032
_reflns_number_total             14778
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00233h2.cif
_cod_data_source_block           mw03045
_cod_original_cell_volume        2976.3(4)
_cod_database_code               4349054
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.806(14) 0.194(14)
2. 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
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C11(H11A,H11B), C10(H10A,H10B), C46(H46A,H46B),
 C19(H19A,H19B), C38(H38A,H38B), C29(H29A,H29B), C47(H47A,H47B), C20(H20A,H20B),
  C28(H28A,H28B), C37(H37A,H37B)
3.b Aromatic/amide H refined with riding coordinates:
 C49(H49), C54(H54), C50(H50), C45(H45), C14(H14), C17(H17), C41(H41),
 C40(H40), C22(H22), C26(H26), C18(H18), C53(H53), C23(H23), C27(H27), C13(H13),
  C36(H36), C31(H31), C32(H32), C35(H35), C44(H44), C9(H9), C4(H4), C8(H8),
 C5(H5)
3.c Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C16(H16A,H16B,H16C), C25(H25A,H25B,H25C), C7(H7A,H7B,
 H7C), C52(H52A,H52B,H52C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              20917
_shelx_hkl_checksum              7718
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 6/14/2013
_olex2_date_sample_submission    6/13/2013
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id MW03045
_olex2_submission_special_instructions 'No special instructions were received'