Reaction of Bis(phosphine)(hydrotris(3,5-dimethylpyrazolyl)borato)rhodium(I) with Phenylacetylene, p-Nitrobenzaldehyde, and Triphenyltin Hydride: Structures of [Rh(Tp*)(PPh3)2], [Rh(Tp*)(H)(C2Ph){P(4-C6H4F)3}], [Rh(Tp*)(H)(COC6H4-4-NO2)(PPh3)], and [Rh(Tp*)(H)(SnPh3)(PPh3)]
Viorel Cîrcu; Manuel A. Fernandes; Laurence Carlton; Inorganic Chemistry 41 (2002) 3859–3865; doi:10.1021/ic0112037

data_4318233
_publ_contact_author             'Laurence Carlton'
_publ_contact_author_email       carlton@aurum.chem.wits.ac.za
_publ_section_title
;
 Reaction of
 Bis(phosphine)(hydrotris(3,5-dimethylpyrazolyl)borato)rhodium(I) with
 Phenylacetylene, p-Nitrobenzaldehyde, and Triphenyltin Hydride:
 Structures of [Rh(Tp*)(PPh3)2], [Rh(Tp*)(H)(C2Ph){P(4-C6H4F)3}],
 [Rh(Tp*)(H)(COC6H4-4-NO2)(PPh3)], and [Rh(Tp*)(H)(SnPh3)(PPh3)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3859
_journal_page_last               3865
_journal_paper_doi               10.1021/ic0112037
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C51 H52 B N6 P2 Rh, C2 H6 O'
_chemical_formula_sum            'C53 H58 B N6 O P2 Rh'
_chemical_formula_weight         970.71
_chemical_name_common
Bis(triphenylphosphine)rhodium(I)hydrotris(3,5-dimethylpyrazolyl)borate
_chemical_name_systematic
;

  ?

;
_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                 112.576(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9664(19)
_cell_length_b                   21.355(3)
_cell_length_c                   20.685(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4880.8(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            33868
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  0.9598
_exptl_absorpt_correction_T_min  0.8556
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'Sheldrick, G. M. (1996). SADABS. University of Gottingen, Germany.'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rhombus
_exptl_crystal_F_000             2024
_exptl_crystal_preparation
'Recrystallised from a 2:1 mixture of CH2Cl2/EtOH'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.319
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         12032
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1237
_reflns_number_gt                7549
_reflns_number_total             12032
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0112037_1.cif
_cod_data_source_block           compound1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4880.8(12)
_cod_database_code               4318233