Acid-base control of hemilabile proton-responsive protecting devices in dimolybdenum, thiolate-bridged complexes.
Le Goff, Alan; Vénec, David; Le Roy, Christine; Pétillon, François Y; Schollhammer, Philippe; Talarmin, Jean; Inorganic chemistry 53 (2014) 2200–2210; doi:10.1021/ic402873c

data_4337209
_publ_section_title
;
 Acid-base control of hemilabile proton-responsive protecting devices in
 dimolybdenum, thiolate-bridged complexes.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2200
_journal_page_last               2210
_journal_paper_doi               10.1021/ic402873c
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C24 H39 B F4 Mo2 N2 O S3'
_chemical_formula_weight         746.44
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_date             2006-07-04T14:58:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 97.331(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0236(3)
_cell_length_b                   12.5884(3)
_cell_length_c                   26.6685(7)
_cell_measurement_reflns_used    12211
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.8669
_cell_measurement_theta_min      2.5753
_cell_volume                     3004.58(15)
_computing_cell_refinement
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        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET)
        (compiled Mar 17 2006,10:57:34)
;
_computing_data_collection
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        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET)
        (compiled Mar 17 2006,10:57:34)
;
_computing_data_reduction
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        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET)
        (compiled Mar 17 2006,10:57:34)
;
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'X-CALIBUR-2 CCD 4-circle diffractometer'
_diffrn_measurement_method
;
omega-scans with kappa -79 deg (chi -58.3 deg), phi 0, 90, 180, 270 deg
;
_diffrn_orient_matrix_UB_11      -0.0236782817
_diffrn_orient_matrix_UB_12      0.0537457057
_diffrn_orient_matrix_UB_13      -0.0000692568
_diffrn_orient_matrix_UB_21      0.0281922411
_diffrn_orient_matrix_UB_22      0.0082797078
_diffrn_orient_matrix_UB_23      -0.023327166
_diffrn_orient_matrix_UB_31      -0.0702057885
_diffrn_orient_matrix_UB_32      -0.0147818007
_diffrn_orient_matrix_UB_33      -0.0132316499
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0484
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_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            25220
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.58
_diffrn_standards_interval_count 50
_exptl_absorpt_coefficient_mu    1.089
_exptl_absorpt_correction_T_max  0.9083
_exptl_absorpt_correction_T_min  0.7359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.29.8 (release 17-03-2006 CrysAlis171 .NET)
        (compiled Mar 17 2006,10:57:34)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.65
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'truncated prism, axis [100]'
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                4290
_reflns_number_total             6150
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402873c_si_002.cif
_cod_data_source_block           altbu2-c
_cod_database_code               4337209