Molecular ordering by halide-halide interactions in dimolybdenum p-halobenzoates
Malcolm H. Chisholm; Christopher B. Durr; Thomas F. Spilker; Philip J. Young; Inorganica Chimica Acta 424 (2015) 300–307; doi:

data_1518974
_publ_section_title
;
 Molecular ordering by halide-halide interactions in dimolybdenum
 p-halobenzoates
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              300
_journal_page_last               307
_journal_volume                  424
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C46 H54 Cl2 Mo2 O8, 2(C4 H8 O)'
_chemical_formula_sum            'C54 H70 Cl2 Mo2 O10'
_chemical_formula_weight         1141.88
_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
_cell_angle_alpha                90
_cell_angle_beta                 115.0250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.5454(3)
_cell_length_b                   28.4540(9)
_cell_length_c                   10.0650(3)
_cell_measurement_reflns_used    6325
_cell_measurement_temperature    152(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_measurement_wavelength     0.71073
_cell_volume                     2736.58(14)
_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-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      152(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0203709
_diffrn_orient_matrix_UB_12      -0.0135478
_diffrn_orient_matrix_UB_13      -0.0939319
_diffrn_orient_matrix_UB_21      -0.1046586
_diffrn_orient_matrix_UB_22      -0.0051866
_diffrn_orient_matrix_UB_23      -0.0176816
_diffrn_orient_matrix_UB_31      -0.0255791
_diffrn_orient_matrix_UB_32      0.0320108
_diffrn_orient_matrix_UB_33      -0.0426193
_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  0.051
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12262
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.438
_diffrn_reflns_theta_min         1.431
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.61
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.534
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.16
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0623P)^2^+2.3166P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1265
_reflns_number_gt                4714
_reflns_number_total             6237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2015-424-300-307-2.cif
_cod_data_source_block           cbd055
_cod_original_cell_volume        2736.57(14)
_cod_database_code               1518974