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_7013009
_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            'C9 H13 B11 Br6 Mo O4'
_chemical_formula_weight         879.50
_chemical_name_common            'H2O Complex'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7520(2)
_cell_length_b                   12.8140(3)
_cell_length_c                   20.1420(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     2516.99(10)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0805
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34957
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.81
_exptl_absorpt_coefficient_mu    10.062
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_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+3.5289*P+(0.0600P)^2^+0.0000sin\q/\l]
where P = 0.00000Fo^2^ + 1.00000Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1009
_reflns_number_gt                5197
_reflns_number_total             5745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303537a.txt
_cod_data_source_block           k01asw19
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' 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 

 Updated bibliographic information.

 Antanas Vaitkus,
 2019-10-03
;
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               7013009