Polar alignment of Λ-shaped basic building units within transition metal oxide fluoride materials.
Holland, Michael; Donakowski, Martin D.; Pozzi, Eric A.; Rasmussen, Andrew M.; Tran, Thanh Thao; Pease-Dodson, Shannon E; Halasyamani, P. Shiv; Seideman, Tamar; Van Duyne, Richard P.; Poeppelmeier, Kenneth R.; Inorganic chemistry 53 (2014) 221–228; doi:10.1021/ic402177j

data_4337516
_publ_section_title
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 Polar alignment of \L-shaped basic building units within transition metal
 oxide fluoride materials.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              221
_journal_page_last               228
_journal_paper_doi               10.1021/ic402177j
_journal_volume                  53
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         '3(F9 Nb2 O2), 2(I), 10(K)'
_chemical_formula_sum            'F27 I2 K10 Nb6 O6'
_chemical_formula_weight         1811.26
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-11-07
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.3471(6)
_cell_length_b                   7.8376(3)
_cell_length_c                   11.6367(3)
_cell_measurement_reflns_used    5498
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      23.98
_cell_measurement_theta_min      2.79
_cell_volume                     1855.73(10)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      299
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0945
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            48327
_diffrn_reflns_theta_full        29.18
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_min         2.00
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.734
_exptl_absorpt_correction_T_max  0.8443
_exptl_absorpt_correction_T_min  0.5125
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Face-Indexed (Sheldrick)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1666
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.037
_refine_diff_density_max         2.432
_refine_diff_density_min         -2.330
_refine_diff_density_rms         0.199
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.10(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         5149
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1088
_reflns_number_gt                3915
_reflns_number_total             5149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402177j_si_007.cif
_cod_data_source_block           Compound_7
_cod_database_code               4337516
_olex2_refinement_description
;
1. Others
 Fixed Sof: I1(0.25) I2(0.25)
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