Fluxional rhodium scorpionate complexes of the hydrotris(methimazolyl)borate (Tm) ligand and their static boratrane derivatives.
López-Gómez, María J; Connelly, Neil G.; Haddow, Mairi F.; Hamilton, Alex; Orpen, A. Guy; Dalton transactions (Cambridge, England : 2003) 39 (2010) 5221–5230; doi:10.1039/c000651c

data_7025422
_publ_section_title
;
 Fluxional rhodium scorpionate complexes of the
 hydrotris(methimazolyl)borate (Tm) ligand and their static boratrane
 derivatives.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5221
_journal_page_last               5230
_journal_paper_doi               10.1039/c000651c
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C31 H31 B N6 O P Rh S3, C H2 Cl2'
_chemical_formula_sum            'C32 H33 B Cl2 N6 O P Rh S3'
_chemical_formula_weight         829.41
_chemical_name_systematic
;
?
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.91(3)
_cell_angle_beta                 85.18(3)
_cell_angle_gamma                67.44(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7020(19)
_cell_length_b                   11.763(2)
_cell_length_c                   16.687(3)
_cell_measurement_reflns_used    908
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      3.35
_cell_volume                     1750.9(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      120(2)
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'fine-slice \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6943
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0883
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17529
_diffrn_reflns_theta_full        30.44
_diffrn_reflns_theta_max         30.44
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.667
_refine_diff_density_min         -1.559
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         9636
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0641
_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 w=1/[\s^2^(Fo^2^)+(0.1158P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1766
_refine_ls_wR_factor_ref         0.1895
_reflns_number_gt                7615
_reflns_number_total             9636
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c000651c.txt
_cod_data_source_block           3
_cod_original_cell_volume        1750.9(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7025422