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_4349050
_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         '2(C18 H41 Co N4 O7 S3), 2(C16 H36 N)'
_chemical_formula_sum            'C68 H154 Co2 N10 O14 S6'
_chemical_formula_weight         1646.22
_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             2015-10-30
_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                 106.650(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5036(15)
_cell_length_b                   25.928(2)
_cell_length_c                   22.811(2)
_cell_measurement_reflns_used    6548
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.011
_cell_measurement_theta_min      2.384
_cell_volume                     9351.7(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_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 0.995
_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  0.0607
_diffrn_reflns_av_unetI/netI     0.0899
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            52521
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.826
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0753 before and 0.0483 after correction.
The Ratio of minimum to maximum transmission is 0.8728.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       needle
_exptl_crystal_F_000             3576
_exptl_crystal_size_max          1.43
_exptl_crystal_size_mid          0.332
_exptl_crystal_size_min          0.322
_refine_diff_density_max         1.191
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         21341
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+2.1452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12581
_reflns_number_total             21341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00233h2.cif
_cod_data_source_block           BuCoBusAq-Z2
_cod_database_code               4349050
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.844
_shelx_estimated_absorpt_t_min   0.510
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H1'D-H1'C
 1.575 with sigma of 0.02
 O1'-H1'D = O1'-H1'C
 0.975 with sigma of 0.02
 H1'C-O3'
 1.78 with sigma of 0.02
 H1C-O7
 1.78 with sigma of 0.02
 O1-H1C
 0.975 with sigma of 0.02
 H1D-O3
 1.777 with sigma of 0.02
 O1-H1D
 0.995 with sigma of 0.02
 C16E-C15D = C16E-C15D
 1.52 with sigma of 0.002
 C4C-C3C = C8C-C7C = C12C-C11C = C16C-C15C
 1.52 with sigma of 0.005
 C16E-C15D \\sim C16E-C15D
 with sigma of 0.005
 C16D-C15D \\sim C16E-C15D
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uiso(H1C) = Uiso(H1D)
4. Rigid body (RIGU) restrains
 N1C, C5C, C1C, C9C, C13C, C6C, C2C, C10C, C14C, C7C, C3C, C11C, C15C, C8C,
 C4C, C12C, C16C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1C, C13C, C14C, C15C, C16C
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 N1D, C13D, C14D, C15D, C16E, C16D
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: H15D(0.5) H15C(0.5) H15B(0.5) H15A(0.5) C16D(0.5) H16G(0.5)
 H16H(0.5) H16I(0.5) C16E(0.5) H16J(0.5) H16K(0.5) H16L(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C1'(H1'A,H1'B), C2'(H2'A,H2'B), C3'(H3'A,H3'B), C4'(H4'A,H4'B), C5'(H5'A,H5'B),
  C6'(H6'A,H6'B), C1D(H1DA,H1DB), C2D(H2DA,H2DB), C3D(H3DA,H3DB), C5D(H5DA,
 H5DB), C6D(H6DA,H6DB), C7D(H7DA,H7DB), C9D(H9DA,H9DB), C10D(H10G,H10H),
 C11D(H11A,H11B), C13D(H13G,H13H), C14D(H14G,H14H), C15D(H15D,H15C), C15D(H15B,
 H15A), C1C(H1CA,H1CB), C2C(H2CA,H2CB), C3C(H3CA,H3CB), C5C(H5CA,H5CB),
 C6C(H6CA,H6CB), C7C(H7CA,H7CB), C9C(H9CA,H9CB), C10C(H10I,H10J), C11C(H11C,
 H11D), C13C(H13I,H13J), C14C(H14I,H14J), C15C(H15E,H15F)
6.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C8'(H8'A,H8'B,H8'C), C9'(H9'A,H9'B,H9'C),
 C10'(H10D,H10E,H10F), C12'(H12D,H12E,H12F), C13'(H13D,H13E,H13F), C14'(H14D,
 H14E,H14F), C16'(H16D,H16E,H16F), C17'(H17D,H17E,H17F), C18'(H18D,H18E,H18F),
 C4D(H4DA,H4DB,H4DC), C8D(H8DA,H8DB,H8DC), C12D(H12G,H12H,H12I), C16D(H16G,H16H,
 H16I), C16E(H16J,H16K,H16L), C4C(H4CA,H4CB,H4CC), C8C(H8CA,H8CB,H8CC),
 C12C(H12J,H12K,H12L), C16C(H16M,H16N,H16O)
;
_shelx_res_checksum              81101
_shelx_hkl_checksum              73095
_shelx_fab_checksum              81032
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 'The crystal was mounted on a loop'
_olex2_submission_original_sample_id CMW-02-139aq
_olex2_submission_special_instructions 'No special instructions were received'