Hydrotris[3-(carboxypyrrolidido)pyrazol-1-yl]borate, the first proven N3O3-hexadentate homoscorpionate ligand
Rheingold, Arnold L.; Incarvito, Christopher D.; Trofimenko, Swiatoslaw; Journal of the Chemical Society, Dalton Transactions  (2000) 1233–; doi:10.1039/b001651i

data_7009518
_publ_section_title
;
 Hydrotris[3-(carboxypyrrolidido)pyrazol-1-yl]borate, the first proven
 N3O3-hexadentate homoscorpionate ligand
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1233
_journal_paper_doi               10.1039/b001651i
_journal_year                    2000
_chemical_formula_sum            'C50 H65 B2 Cl5 F6 N18 Nd O6 P'
_chemical_formula_weight         1502.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.9329(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.0247(4)
_cell_length_b                   19.8463(3)
_cell_length_c                   26.3284(4)
_cell_measurement_temperature    173(2)
_cell_volume                     13198.4(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            27637
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    1.090
_exptl_absorpt_correction_T_max  0.6696
_exptl_absorpt_correction_T_min  0.6696
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6104
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         2.467
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     842
_refine_ls_number_reflns         12673
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      2.045
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0852
_refine_ls_shift/su_max          0.093
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2425
_refine_ls_wR_factor_ref         0.2638
_reflns_number_gt                10448
_reflns_number_total             12673
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001651i.txt
_cod_data_source_block           trof87
_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 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        13198.4(5)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7009518