An unprecedented κ2N,H bonding mode for a hydridotris(pyrazolyl)borato ligand
Malbosc, François; Kalck, Philippe; Daran, Jean-Claude; Etienne, Michel; Journal of the Chemical Society, Dalton Transactions  (1999) 271–; doi:10.1039/a809323g

data_7027200
_publ_section_title
;
 An unprecedented \k2N,H bonding mode for a hydridotris(pyrazolyl)borato
 ligand
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              271
_journal_paper_doi               10.1039/a809323g
_journal_year                    1999
_chemical_compound_source        'synthetic route'
_chemical_formula_moiety         ' C42 H45 Rh1 P2 CL3 O1 N6 B1 '
_chemical_formula_sum            'C42 H45 B Cl3 N6 O P2 Rh'
_chemical_formula_weight         931.88
_chemical_melting_point          ?
_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
_cell_angle_alpha                101.073(18)
_cell_angle_beta                 102.282(19)
_cell_angle_gamma                92.460(19)
_cell_formula_units_Z            2
_cell_length_a                   11.1644(19)
_cell_length_b                   12.0058(19)
_cell_length_c                   17.097(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      24.25
_cell_measurement_theta_min      1.77
_cell_volume                     2189.1(7)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'CAMERON (Watkin, Prout & Pearce, 1996)'
_computing_publication_material  'CRYSTALS Issue 10 (Watkin et al., 1996)'
_computing_structure_refinement  'CRYSTALS Issue 10 (Watkin et al., 1996)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      180(2)
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '/f scan'
_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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17587
_diffrn_reflns_theta_max         24.25
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_time  'every frame'
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.6785
_exptl_absorpt_correction_T_max  0.7748
_exptl_absorpt_correction_T_min  0.3603
_exptl_absorpt_correction_type   empirical(DIFABS)
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       box
_exptl_crystal_F_000             955
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.462
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_obs   1.0112
_refine_ls_hydrogen_treatment
;
 H atoms placed geometrically after each cycle, but those attached to
 the methyl groups of the phosphines were refined with an equivalent
 isotropic thermal parameter.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         5120
_refine_ls_R_factor_obs          0.0407
_refine_ls_shift/su_max          0.074031
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
; 
 Robust-resistant weighting scheme (Prince E, 1982): 
 w=y[1-(\DF/6\s(Fo^2^)]^2^' where y=1/\SArTr(x) with 3 coefficients 
 Ar(2.34, -0.0136, 1.94) for the Chebyshev polynomial ArTr(x) where 
 x was Fc/Fc(max).
;
_refine_ls_wR_factor_obs         0.0425
_reflns_number_gt                5120
_reflns_number_total             6532
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            809323gsup1.cif
_cod_data_source_block           3a
_cod_depositor_comments
;
 Changing the _chemical_formula_sum data item value from
 'C43 H45 B L3 N6 O P2 Rh' to 'C42 H45 B Cl3 N6 O P2 Rh'.

 Antanas Vaitkus,
 2017-01-15

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_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:

'_atom_sites_solution_primary' value 'Direct_Methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'Geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        2189.1(6)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C42 H45 Rh1 P2 CL3 O1 N6 B1 '
_cod_database_code               7027200