Isolation, Characterization, and Computational Studies of the Novel [Mo3(μ3-Br)2(μ-Br)3Br6]2- Cluster Anion
Patrina Paraskevopoulou; Christodoulos Makedonas; Nikolaos Psaroudakis; Christiana A. Mitsopoulou; Georgios Floros; Andriana Seressioti; Marinos Ioannou; Yiannis Sanakis; Nigam Rath; Carlos J. Gómez García; Pericles Stavropoulos; Konstantinos Mertis; Inorganic Chemistry 49 (2010) 2068–2076; doi:10.1021/ic901432j

data_4314944
_publ_section_title
;
 Isolation, Characterization, and Computational Studies of the Novel
 [Mo3(\m3-Br)2(\m-Br)3Br6]2- Cluster Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2068
_journal_page_last               2076
_journal_paper_doi               10.1021/ic901432j
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C32 H72 Br11 Mo3 N2'
_chemical_formula_weight         1651.75
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.348(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.077(2)
_cell_length_b                   11.8638(11)
_cell_length_c                   22.521(2)
_cell_measurement_reflns_used    4297
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.27
_cell_measurement_theta_min      2.39
_cell_volume                     5061.3(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_sigmaI/netI    0.0909
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26806
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    9.440
_exptl_absorpt_correction_T_max  0.4520
_exptl_absorpt_correction_T_min  0.1163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs v2008/1'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.168
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3156
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.339
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4442
_refine_ls_number_restraints     404
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.1986
_reflns_number_gt                2588
_reflns_number_total             4442
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901432j_si_001.cif
_cod_data_source_block           p12208
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'no' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        5061.3(9)
_cod_database_code               4314944