A tris(pyrazolyl)borate rhodium phosphite complex that undergoes an Arbusov-like rearrangement
Jiao, Yunzhe; Brennessel, William W.; Jones, William D.; Acta Crystallographica Section C 69 (2013) 939–942; doi:10.1107/S0108270113015953

data_2019150
_publ_section_title
;
 A tris(pyrazolyl)borate rhodium phosphite complex that undergoes an
 Arbusov-like rearrangement
;
_journal_coeditor_code           YP3031
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              939
_journal_page_last               942
_journal_paper_doi               10.1107/S0108270113015953
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Rh2 (C H3)2 (C2 H6 O3 P)2 (C15 H22 B N6)2]'
_chemical_formula_moiety         'C36 H62 B2 N12 O6 P2 Rh2'
_chemical_formula_sum            'C36 H62 B2 N12 O6 P2 Rh2'
_chemical_formula_weight         1048.35
_chemical_name_common            jonyj40
_chemical_name_systematic
'Bis(\m-dimethyl phosphito)-\k^2^<i>P</i>:<i>O</i>;\k^2^<i>O</i>:<i>P</i>-bis{methyl[tris(3,5,-dimethyl-1<i>H</i>-pyrazol-1-yl-\k<i>N</i>^2^)borato]rhodium(III)}'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                71.919(2)
_cell_angle_beta                 88.912(2)
_cell_angle_gamma                67.725(2)
_cell_formula_units_Z            1
_cell_length_a                   10.1383(9)
_cell_length_b                   10.6676(10)
_cell_length_c                   13.5193(13)
_cell_measurement_reflns_used    4044
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      29.11
_cell_measurement_theta_min      2.18
_cell_volume                     1278.1(2)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39087
_diffrn_reflns_theta_full        33.730
_diffrn_reflns_theta_max         33.728
_diffrn_reflns_theta_min         2.184
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
 Highly disordered solvent was located in channels parallel to the
 b-axis. Reflection contributions from this solvent were removed
 using program PLATON, function SQUEEZE (Spek, 2003), which determined
 there to be 96 electrons in 250 \%A^3^ removed per unit cell. Since
 the exact identity and amount of solvent could not be determined,
 no solvent was included in the atom list or molecular formula. (One
 set of residual peaks did appear to be n-pentane, disordered over an
 inversion center. However, this did not define the entire solvent
 area.) Thus all reported items that derive from the molecular formula
 (e.g., F(000), density, molecular weight, etc.) are known to be
 incorrect.
;
_refine_diff_density_max         4.569
_refine_diff_density_min         -1.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         10151
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0832P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1570
_reflns_number_gt                7079
_reflns_number_total             10151
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yp3031.cif
_cod_data_source_block           I
_cod_database_code               2019150
_cod_database_fobs_code          2019150
_shelx_estimated_absorpt_t_min   0.851
_shelx_estimated_absorpt_t_max   0.914
_shelx_res_checksum              19898
_shelxl_version_number           .000002012