Bis[hydrotris(pyrazol-1-yl)borato]titanium(II): a stable Tp2M complex of singular reactivity.
Kayal, A.; Kuncheria, J.; Lee, S. C.; Chemical communications (Cambridge, England)  (2001) 2482–2483; doi:10.1039/b108115b

data_7125520
_publ_section_title
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 Bis[hydrotris(pyrazol-1-yl)borato]titanium(II): a stable Tp2M complex of
 singular reactivity.
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_journal_issue                   23
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2482
_journal_page_last               2483
_journal_paper_doi               10.1039/b108115b
_journal_year                    2001
_chemical_formula_moiety         'C36 H40 B4 N24 O Ti2, 4(C6 H6)'
_chemical_formula_sum            'C60 H64 B4 N24 O Ti2'
_chemical_formula_weight         1276.39
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.5983(6)
_cell_length_b                   15.6270(6)
_cell_length_c                   20.2307(8)
_cell_measurement_reflns_used    27250
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.14
_cell_measurement_theta_min      1.64
_cell_volume                     6512.1(4)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       NONIUS-COLLECT
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SIEMENS SHELXTL'
_computing_publication_material  'SIEMENS SHELXTL'
_computing_structure_refinement  'SIEMENS SHELXTL'
_computing_structure_solution    'SIEMENS SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0859
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27250
_diffrn_reflns_theta_max         24.14
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.48(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.008
_refine_ls_goodness_of_fit_obs   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         9955
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.008
_refine_ls_restrained_S_obs      1.057
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_obs          0.0483
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+0.4022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0970
_refine_ls_wR_factor_obs         0.0843
_reflns_number_observed          7077
_reflns_number_total             9955
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            b108115b.txt
_cod_data_source_block           '[(k2-Tp)(K3-Tp)Ti]2(mu-O).4C6H6'
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+0.4022P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+0.4022P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_database_code               7125520