Synthesis, Structure, and Properties of Group 4 and 5 Metal Pyrazolato Chloride Complexes
Carlos Yélamos; Mary Jane Heeg; Charles H. Winter; Inorganic Chemistry 38 (1999) 1871–1878; doi:10.1021/ic981096p

data_4321911
_publ_section_title
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 Synthesis, Structure, and Properties of Group 4 and 5 Metal Pyrazolato
 Chloride Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1871
_journal_page_last               1878
_journal_paper_doi               10.1021/ic981096p
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C33 H57 Cl2 N6 Nb'
_chemical_formula_weight         701.66
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.3280(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2051(3)
_cell_length_b                   38.3650(12)
_cell_length_c                   9.7585(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    295(2)
_cell_volume                     3814.2(2)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Siemens P4/CCD'
_diffrn_measurement_method       'SMART CCD'
_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  0.051
_diffrn_reflns_av_sigmaI/netI    0.0753
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            22170
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    0.484
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            P2(1)/c
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       'rods and plates'
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.00000(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.006
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         8140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_restrained_S_obs      1.092
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_obs          0.0498
_refine_ls_shift/esd_max         -2.160
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1167
_refine_ls_wR_factor_obs         0.0985
_reflns_number_observed          5525
_reflns_number_total             8141
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981096p_3.cif
_cod_data_source_block           niob(9)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.0000P] 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^)+(0.0523P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4321911