(Acetylacetonato-κ^2^<i>O</i>,<i>O</i>')dichloridobis(methanolato-κ<i>O</i>)niobium(V)
Herbst, Leandra; Visser, Hendrik G.; Roodt, Andreas; Pretorius, Carla; Acta Crystallographica Section E 68 (2012) m1392–; doi:10.1107/S1600536812042638

data_2236134
_publ_section_title
;
 (Acetylacetonato-\k^2^<i>O</i>,<i>O</i>')dichloridobis(methanolato-\k<i>O</i>)niobium(V)
;
_journal_coeditor_code           BT6846
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1392
_journal_paper_doi               10.1107/S1600536812042638
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Nb (C H3 O)2 (C5 H7 O2) Cl2]'
_chemical_formula_moiety         'C7 H13 Cl2 Nb O4'
_chemical_formula_sum            'C7 H13 Cl2 Nb O4'
_chemical_formula_weight         324.98
_chemical_name_systematic
;
(Acetylacetonato-\k^2^<i>O</i>,<i>O</i>')dichloridobis(methanolato-
\k<i>O</i>)niobium(V)
;
_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           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 111.2790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7985(2)
_cell_length_b                   11.6028(3)
_cell_length_c                   14.6819(2)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.88
_cell_measurement_theta_min      2.3
_cell_volume                     1237.91(5)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2004)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2004)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25521
_diffrn_reflns_theta_full        28
_diffrn_reflns_theta_max         28
_diffrn_reflns_theta_min         2.3
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.391
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2004)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubiod
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.384
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.898
_refine_diff_density_min         -1.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.027
_refine_ls_R_factor_gt           0.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0177P)^2^+2.6018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0602
_reflns_number_gt                2873
_reflns_number_total             2995
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            bt6846.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2236134
_cod_database_fobs_code          2236134