Femtosecond Study of Dimolybdenum Paddlewheel Compounds with Amide/Thioamide Ligands: Symmetry, Electronic Structure, and Charge Distribution in the (1)MLCT S1 State.
Jiang, Changcheng; Young, Philip J.; Brown-Xu, Samantha; Gallucci, Judith C.; Chisholm, Malcolm H.; Inorganic chemistry 56 (2017) 1433–1445; doi:10.1021/acs.inorgchem.6b02517

data_4345479
_publ_section_title
;
 Femtosecond Study of Dimolybdenum Paddlewheel Compounds with
 Amide/Thioamide Ligands: Symmetry, Electronic Structure, and Charge
 Distribution in the (1)MLCT S1 State.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1433
_journal_page_last               1445
_journal_paper_doi               10.1021/acs.inorgchem.6b02517
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C65.40 H73.40 Mo2 N2 O7 S0.30'
_chemical_formula_sum            'C65.4 H73.4 Mo2 N2 O7 S0.3'
_chemical_formula_weight         1200.95
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2016-03-16T16:43:36-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.2710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6467(4)
_cell_length_b                   15.3031(4)
_cell_length_c                   24.6547(6)
_cell_measurement_reflns_used    14517
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_measurement_wavelength     0.71073
_cell_volume                     6243.1(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_orient_matrix_UB_11      0.004212
_diffrn_orient_matrix_UB_12      -0.047961
_diffrn_orient_matrix_UB_13      0.027714
_diffrn_orient_matrix_UB_21      -0.058971
_diffrn_orient_matrix_UB_22      -0.012473
_diffrn_orient_matrix_UB_23      -0.008677
_diffrn_orient_matrix_UB_31      0.012526
_diffrn_orient_matrix_UB_32      -0.042594
_diffrn_orient_matrix_UB_33      -0.028665
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            77304
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.451
_diffrn_reflns_theta_min         2.129
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2498
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.31
_platon_squeeze_details
;TITL shelx     P 21/c       R = 0.05
CELL   16.6467   15.3031   24.6547     90.00     96.27     90.00
SPGR P21/c
C101 0.969 0.502 0.072 !       2.55 eA-3
C102 0.968 0.533 0.034 !       2.10 eA-3
C103 0.042 0.975 0.485 !       1.79 eA-3
C104 1.000 0.972 0.479 !       1.70 eA-3
C105 1.001 0.423 0.003 !       1.56 eA-3
Q106 0.303 0.993 0.156 !       0.89 eA-3
Q107 0.667 0.997 0.384 !       0.83 eA-3
Q108 0.183 0.982 0.118 !       0.78 eA-3
Q109 0.063 0.997 0.078 !       0.75 eA-3
Q110 0.234 1.003 0.142 !       0.72 eA-3
Q111 0.488 0.469 0.293 !       0.71 eA-3
Q112 0.871 0.965 0.187 !       0.68 eA-3
Q113 0.247 0.953 0.134 !       0.66 eA-3
Q114 0.487 0.434 0.334 !       0.65 eA-3
Q115 0.786 0.999 0.421 !       0.63 eA-3
Q116 0.828 0.044 0.225 !       0.59 eA-3
Q117 0.577 0.483 0.733 !       0.58 eA-3
Q118 0.423 0.517 0.267 !       0.58 eA-3
Q119 0.494 0.905 0.221 !       0.55 eA-3
Q120 0.252 0.999 0.119 !       0.55 eA-3
Q121 0.190 0.494 0.339 !       0.54 eA-3
Q122 0.887 1.001 0.225 !       0.52 eA-3
;
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     746
_refine_ls_number_reflns         14205
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+3.4095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0966
_reflns_number_gt                11032
_reflns_number_total             14205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02517_si_002.cif
_cod_data_source_block           Chisholm2054
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C65.40 H73.40 Mo2 N2 O7 S0.30'
_cod_database_code               4345479
_platon_squeeze_void_probe_radius 1.20