Molybdenum Complexes of an Eight-Electron-Donor Monocarbollide Ligand, Geometrically Constrained by Intramolecular Five-Membered-Ring Formation
Kautz, Jason A.; Kissounko, Denis A.; Kissounko, Natalia S.; Stone, F. Gordon A.; Organometallics 21 (2002) 2547–; doi:10.1021/om020103l

data_4076835
_publ_section_title
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 Molybdenum Complexes of an Eight-Electron-Donor Monocarbollide Ligand,
 Geometrically Constrained by Intramolecular Five-Membered-Ring Formation
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2547
_journal_paper_doi               10.1021/om020103l
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C10 H21 B10 Mo N O5'
_chemical_formula_weight         439.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.100(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3159(7)
_cell_length_b                   9.8420(12)
_cell_length_c                   15.0004(16)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      24.0
_cell_measurement_theta_min      20.0
_cell_volume                     1964.6(3)
_computing_cell_refinement       'Enraf-Nonius CAD4 (1989)'
_computing_data_collection       'Enraf-Nonius CAD4 (1989)'
_computing_data_reduction        'XCAD4 Siemens Software (Harms, 1993)'
_computing_molecular_graphics    'XP in SHELXTL-PC (Bruker, 1995)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w-2\q
_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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4728
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        6.08
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular blocks'
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.7423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                3427
_reflns_number_total             4501
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020103l.cif
_cod_data_source_block           2
_cod_depositor_comments
;
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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.7423P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.7423P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4076835