Oxidation Chemistry of Axially Protected Mo2 and W2 Quadruply Bonded Compounds
Michael Nippe; Eric Victor; John F. Berry; Inorganic Chemistry 48 (2009) 11889–11895; doi:10.1021/ic901965b

data_4303933
_publ_section_title
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Oxidation Chemistry of Axially Protected Mo2 and W2 Quadruply Bonded Compounds
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11889
_journal_page_last               11895
_journal_paper_doi               10.1021/ic901965b
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C40 H32 N12 W2, C24 H20 B'
_chemical_formula_sum            'C64 H52 B N12 W2'
_chemical_formula_weight         1367.69
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 90.388(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.9775(7)
_cell_length_b                   27.614(2)
_cell_length_c                   10.7148(8)
_cell_measurement_reflns_used    9251
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.5463
_cell_measurement_theta_min      2.2686
_cell_volume                     2656.2(3)
_computing_cell_refinement       'SAINT Ver. 6.22  (Bruker-AXS, 2003)'
_computing_data_collection       'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT Ver. 6.22'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker CCD-1000 area detector'
_diffrn_measurement_method       '0.30\% \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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32806
_diffrn_reflns_theta_full        29.58
_diffrn_reflns_theta_max         29.58
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    4.383
_exptl_absorpt_correction_T_max  0.4283
_exptl_absorpt_correction_T_min  0.1998
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            darkpurple
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1346
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.677
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.199
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         13938
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.0467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0562
_reflns_number_gt                13757
_reflns_number_total             13938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901965b_si_001_3.cif
_cod_data_source_block           1BPh4(P2(1))
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_cell_volume        2656.2(4)
_cod_database_code               4303933