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_4337509
_publ_section_title
;
 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(F7 Mo2 O4), 2(Br), 10(K)'
_chemical_formula_sum            'Br2 F21 K10 Mo6 O12'
_chemical_formula_weight         1717.46
_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             2012-11-15
_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                   20.0790(6)
_cell_length_b                   7.7580(2)
_cell_length_c                   11.4836(3)
_cell_measurement_reflns_used    2898
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      35.51
_cell_measurement_theta_min      3.76
_cell_volume                     1788.83(8)
_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
;
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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.739
_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  0.0000
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5391
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         38.66
_diffrn_reflns_theta_min         2.03
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.587
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.4939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/4 (Bruker,2010) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0687 before and 0.0464 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0642 before and 0.0460 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 3:
 wR2(int) was 0.0821 before and 0.0512 after correction.
 The Ratio of minimum to maximum transmission is 0.79.
 The \l/2 correction factor is Not present
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1594
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.044
_refine_diff_density_max         3.989
_refine_diff_density_min         -4.609
_refine_diff_density_rms         0.340
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         6426
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.231
_refine_ls_R_factor_all          0.0467
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1421
_reflns_number_gt                6167
_reflns_number_total             5391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402177j_si_006.cif
_cod_data_source_block           Compound_6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               4337509
_olex2_refinement_description
;
1. Shared sites
{F1, O1}
{F3, O3}
{F4, O4}
{F5, O5}
{F6, O6}
{F7, O7}
{F8, O8}
{F10, O10}
{F11, O11}
{F12, O12}
{F13, O13}
{F15, O15}
2. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(O1)
Uanis(F3) = Uanis(O3)
Uanis(F4) = Uanis(O4)
Uanis(F5) = Uanis(O5)
Uanis(F6) = Uanis(O6)
Uanis(F7) = Uanis(O7)
Uanis(F8) = Uanis(O8)
Uanis(F10) = Uanis(O10)
Uanis(F11) = Uanis(O11)
Uanis(F12) = Uanis(O12)
Uanis(F13) = Uanis(O13)
Uanis(F15) = Uanis(O15)
3. Others
 Fixed Sof: Br1(0.25) Br3(0.25) F1(0.75) F3(0.75) F4(0.75) F5(0.75) F6(0.75)
 F7(0.75) F8(0.75) F10(0.75) F11(0.75) F12(0.75) F13(0.75) F15(0.75) O1(0.25)
 O3(0.25) O4(0.25) O5(0.25) O6(0.25) O7(0.25) O8(0.25) O10(0.25) O11(0.25)
 O12(0.25) O13(0.25) O15(0.25)
;