A Chiral Alkyltris(pyrazolyl)borate Ligand: Synthesis of [(Ipc)B(pz)3Mn(CO)3] and [(Ipc)B(pz)3Ru(p-cymene)]PF6 (Ipc = Isopinocampheyl)
Philip J. Bailey; Pedro Pinho; Simon Parsons; Inorganic Chemistry 42 (2003) 8872–8877; doi:10.1021/ic035061n

data_4312834
_publ_section_title
;
 A Chiral Alkyltris(pyrazolyl)borate Ligand: Synthesis of
 [(Ipc)B(pz)3Mn(CO)3] and [(Ipc)B(pz)3Ru(p-cymene)]PF6 (Ipc =
 Isopinocampheyl)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8872
_journal_page_last               8877
_journal_paper_doi               10.1021/ic035061n
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         '[Mn(CO)3(pbBpz)]'
_chemical_formula_sum            'C22 H26 B Mn N6 O3'
_chemical_formula_weight         488.24
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           1
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                60.555(3)
_cell_angle_beta                 63.211(3)
_cell_angle_gamma                62.917(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0130(18)
_cell_length_b                   11.6451(19)
_cell_length_c                   11.6288(19)
_cell_measurement_reflns_used    1850
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     1105.7(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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    Dirdif
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.862
_diffrn_measured_fraction_theta_max 0.862
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0864
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5836
_diffrn_reflns_theta_full        28.83
_diffrn_reflns_theta_max         28.83
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Twinabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         5836
_refine_ls_number_restraints     709
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1334
_reflns_number_gt                4695
_reflns_number_total             5836
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035061nsi20030909_102546_1.cif
_cod_data_source_block           ppp104
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'Multiscan'
changed to 'multi-scan' 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_database_code               4312834