Oxidative stretching of metal-metal bonds to their limits.
Brogden, David W.; Turov, Yevgeniya; Nippe, Michael; Li Manni, Giovanni; Hillard, Elizabeth A.; Clérac, Rodolphe; Gagliardi, Laura; Berry, John F.; Inorganic chemistry 53 (2014) 4777–4790; doi:10.1021/ic5007204

data_4338161
_publ_section_title
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 Oxidative stretching of metal-metal bonds to their limits.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4777
_journal_page_last               4790
_journal_paper_doi               10.1021/ic5007204
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C40 H32 Cr2 N12, 2(C F3 O3 S)'
_chemical_formula_sum            'C42 H32 Cr2 F6 N12 O6 S2'
_chemical_formula_weight         1082.92
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 108.1919(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.5721(5)
_cell_length_b                   8.8060(2)
_cell_length_c                   22.5134(5)
_cell_measurement_temperature    100(2)
_cell_volume                     4251.31(17)
_computing_cell_refinement       'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_computing_data_collection       'APEX2 Ver. 2013.2-0 (Bruker-AXS, 2013)'
_computing_data_reduction        'SAINT+ Ver. 8.30C (Bruker-AXS, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008-2013)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2013)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  Gromit
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            78408
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.75
_diffrn_reflns_theta_min         1.90
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  0.7331
_exptl_absorpt_correction_T_min  0.6610
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2009/1 (Bruker,2010) was used for absorption correction.
wR2(int) was 0.1139 before and 0.0617 after correction.
The Ratio of minimum to maximum transmission is 0.9017.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         8122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+8.4844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                6141
_reflns_number_total             8122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5007204_si_001.cif
_cod_data_source_block           berry204
_cod_depositor_comments
'Adding full bibliography for 4338161--4338168.cif.'
_cod_original_cell_volume        4251.31(16)
_cod_database_code               4338161
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: F5(0.46696) F6(0.46696) O4(0.46696) O6(0.46696) F5A(0.53304)
 F6A(0.53304) O4A(0.53304) O6A(0.53304)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C40(H40)
;