A Novel Layered Niobium Oxychloride Compound Based on Nb2 Pairs and Nb6 Octahedral Clusters: Synthesis and Crystal and Electronic Structures of Nb10Cl16O7
Stéphane Cordier; Fakhili Gulo; Thierry Roisnel; Régis Gautier; Boris le Guennic; Jean François Halet; Christiane Perrin; Inorganic Chemistry 42 (2003) 8320–8327; doi:10.1021/ic0350990

data_4312740
_publ_contact_author_address
;
LCSIM UMR 6511 CNRS - Universit\'e de Rennes 1, Institut de Chimie
de Rennes, B\^at. 10A, Campus de Beaulieu, Avenue du G\'en\'eral Leclerc,
35042 Rennes, France
;
_publ_contact_author_email       stephane.cordier@univ-rennes1.fr
_publ_contact_author_fax         33299635704
_publ_contact_author_name        'Cordier, Stephane'
_publ_contact_author_phone       33223236253
_publ_section_title
;
 A Novel Layered Niobium Oxychloride Compound Based on Nb2 Pairs and Nb6
 Octahedral Clusters: Synthesis and Crystal and Electronic Structures of
 Nb10Cl16O7
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8320
_journal_page_last               8327
_journal_paper_doi               10.1021/ic0350990
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'Cl16 Nb10 O7'
_chemical_formula_sum            'Cl16 Nb10 O7'
_chemical_formula_weight         1608.3
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2003-04-29
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 121.243(5)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   17.646(5)
_cell_length_b                   3.264(5)
_cell_length_c                   12.893(5)
_cell_measurement_reflns_used    853
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_volume                     634.9(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            1387
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    6.044
_exptl_absorpt_correction_T_max  0.8246
_exptl_absorpt_correction_T_min  0.4526
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.936
_refine_ls_extinction_coef       0.0016(3)
_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_ref   1.217
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.6585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0828
_reflns_number_gt                756
_reflns_number_total             855
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0350990si20030917_110023.cif
_cod_data_source_block           c2m
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4312740