Investigation of the synthesis of {Mo(η5-C5H5)(CO)3}+ fragments partnered with the monoanionic carboranes [closo-CB11H11Br]-, [closo-CB11H6Br6]- and [closo-HCB11Me11]- by silver salt metathesis and hydride abstraction
Patmore, Nathan J.; Ingleson, Michael J.; Mahon, Mary F.; Weller, Andrew S.; Dalton Transactions  (2003) 2894–2904; doi:10.1039/b303537a

data_7013007
_publ_section_title
;
 Investigation of the synthesis of {Mo(\h5-C5H5)(CO)3}+ fragments
 partnered with the monoanionic carboranes [closo-CB11H11Br]-,
 [closo-CB11H6Br6]- and [closo-HCB11Me11]- by silver salt metathesis
 and hydride abstraction
;
_journal_coden_ASTM              DTARAF
_journal_issue                   14
_journal_name_full               'Dalton Transactions'
_journal_page_first              2894
_journal_page_last               2904
_journal_paper_doi               10.1039/b303537a
_journal_year                    2003
_chemical_formula_sum            'C31 H49 B11'
_chemical_formula_weight         540.61
_chemical_name_common            6
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.048(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5600(8)
_cell_length_b                   22.7370(14)
_cell_length_c                   15.3050(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     3308.3(4)
_computing_data_reduction
'Denzo and Scalepack (otwinowski & Minor, 1997'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.787
_diffrn_measured_fraction_theta_max 0.787
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       KappaCCD
_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  0.1147
_diffrn_reflns_av_sigmaI/netI    0.1675
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11411
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    0.056
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0016(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1688
_refine_ls_R_factor_gt           0.0758
_refine_ls_shift/su_max          0.329
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
[1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/
[\s^2^(Fo^2^)+0.0000+0.8129*P+(0.0790P)^2^+0.0000sin\q/\l]
where P = 0.00000Fo^2^ + 1.00000Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.2194
_reflns_number_gt                3073
_reflns_number_total             6020
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303537a.txt
_cod_data_source_block           k02asw10
_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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'PSI-Scans' was replaced
with 'psi-scan' value.

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

 Updated bibliographic information.

 Antanas Vaitkus,
 2019-10-03
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7013007