Boron Functionalization of Bis(pyrazolyl)borate Ligands: Molecular Structures of [RuX(PPh3)2{(MeO)2B(pz)2}] (X = H, Cl; pz = pyrazol-1-yl)
Abernethy, Robyn J.; Hill, Anthony F.; Smith, Matthew K.; Willis, Anthony C.; Organometallics 28 (2009) 6152–; doi:10.1021/om9006592

data_4070213
_publ_section_title
;
 Boron Functionalization of Bis(pyrazolyl)borate Ligands: Molecular
 Structures of [RuX(PPh3)2{(MeO)2B(pz)2}] (X = H, Cl; pz = pyrazol-1-yl)
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6152
_journal_paper_doi               10.1021/om9006592
_journal_volume                  28
_journal_year                    2009
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C44 H43 B N4 O2 P2 Ru , 2(C H2 Cl2)'
_chemical_formula_sum            'C46 H47 B Cl4 N4 O2 P2 Ru'
_chemical_formula_weight         1003.54
_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
_audit_creation_date             04-20-04
_audit_creation_method           CRYSTALS_ver_12-03-99
_audit_update_record
;
2004-04-21 - Report on C46 H47 B1 Cl4 N4 O2 P2 Ru1 
             by Anthony C. Willis
             for   Anthony F. Hill and Robyn Abernethy

2004-04-21 - passes checkcif tests with minor warnings

;
_cell_angle_alpha                90
_cell_angle_beta                 97.9591(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.94920(10)
_cell_length_b                   21.8625(2)
_cell_length_c                   17.7095(2)
_cell_measurement_reflns_used    67768
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     4581.85(8)
_computing_cell_refinement
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
 COLLECT (Nonius BV, 1997) 
;
_computing_data_reduction
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_molecular_graphics
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2003) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2003) 
;
_computing_structure_solution
; 
 SIR92 (Altomare et al, 1994) 
;
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
; 
Nonius Kappa CCD 
;
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.04
_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       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            92804
_diffrn_reflns_theta_full        27.476
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         2.689
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.56
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         6225
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.000748
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.601 0.308 0.344 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0419
_refine_ls_wR_factor_gt          0.0348
_refine_ls_wR_factor_ref         0.0348
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                6225
_reflns_number_total             10486
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            om9006592_si_001.cif
_cod_data_source_block           rja8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 1715 2011-07-08 13:25:40Z adriana 

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 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C46 H47 B Cl4 N4 O2 P2 Ru '
_cod_database_code               4070213