Designer clusters: synthesis and characterization of Cp*2Rh2Co3(CO)8B3HCl (Cp* =η5-C5Me5)
Lei, Xinjian; Shang, Maoyu; Fehlner, Thomas P.; Chemical Communications  (1999) 933–; doi:10.1039/a901491h

data_7110499
_publ_section_title
;
 Designer clusters: synthesis and characterization of Cp*2Rh2Co3(CO)8B3HCl
 (Cp* =\h5-C5Me5)
;
_journal_issue                   10
_journal_name_full               'Chemical Communications'
_journal_page_first              933
_journal_paper_doi               10.1039/a901491h
_journal_year                    1999
_chemical_formula_sum            'C28 H31 B3 Cl Co3 O8 Rh2'
_chemical_formula_weight         946.02
_chemical_name_systematic
;
{(Cp*Rh)2}{Co3(CO)8}(BBH)(BCl)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                88.104(10)
_cell_angle_beta                 77.308(14)
_cell_angle_gamma                62.825(11)
_cell_formula_units_Z            2
_cell_length_a                   9.4979(15)
_cell_length_b                   9.4931(13)
_cell_length_c                   21.394(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     1669.1(5)
_computing_cell_refinement       'CAD4 (Enraf-Nonius, 1985)'
_computing_data_collection       'CAD4 (Enraf-Nonius, 1985)'
_computing_data_reduction
;
XCAD4 (Harms, 1996)
SHEXTL-V5 (Siemens, 1994)
;
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHEXTL-V5 (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       '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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5874
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.553
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6178
_exptl_absorpt_correction_type   Difabs
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'Irregular Polyhedron'
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.036
_refine_ls_goodness_of_fit_obs   1.081
_refine_ls_hydrogen_treatment
;
Borane hydrogen atom was isotropically refined with bond lengthen restraint,
hydrogen atoms of methyl groups were refined with riding model.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         5874
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_restrained_S_obs      1.081
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_obs          0.0348
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+1.3481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0884
_refine_ls_wR_factor_obs         0.0821
_reflns_number_observed          4737
_reflns_number_total             5874
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            901491hsup1.cif
_cod_data_source_block           f9802
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+1.3481P] 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^)+(0.0502P)^2^+1.3481P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1669.1(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110499