New H-bond accepting tris(pyrazolyl)borates: stabilization of metal aquo species as models for the vicinal oxygen chelate enzyme superfamily
Hammes, Brian S.; Carrano, Mary W.; Carrano, Carl J.; Journal of the Chemical Society, Dalton Transactions  (2001) 1448–; doi:10.1039/b009621k

data_7010481
_publ_section_title
;
 New H-bond accepting tris(pyrazolyl)borates: stabilization of metal
 aquo species as models for the vicinal oxygen chelate enzyme
 superfamily
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1448
_journal_paper_doi               10.1039/b009621k
_journal_year                    2001
_chemical_formula_sum            'C21 H34 B Cl N6 Ni O13'
_chemical_formula_weight         683.51
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.378(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.419(2)
_cell_length_b                   18.220(2)
_cell_length_c                   18.1663(15)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.51
_cell_measurement_theta_min      5.37
_cell_volume                     3112.2(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w 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  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4316
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.17
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_F_000             1424
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.976
_refine_ls_goodness_of_fit_obs   0.978
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         4027
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.976
_refine_ls_restrained_S_obs      0.975
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_obs          0.0525
_refine_ls_shift/esd_max         0.078
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0937P)^2^+5.9086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1615
_refine_ls_wR_factor_obs         0.1391
_reflns_number_observed          3085
_reflns_number_total             4028
_reflns_observed_criterion       2sigma(I)
_cod_data_source_file            b009621k.txt
_cod_data_source_block           bsh77
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0937P)^2^+5.9086P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0937P)^2^+5.9086P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3112.1(7)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7010481