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_4337514
_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         '4(F7 Mo2 O4), F14.02 Mo4 O8, 2(Cl), 20(K)'
_chemical_formula_sum            'Cl2 F42.02 K20 Mo12 O24'
_chemical_formula_weight         3186.56
_chemical_name_systematic
;
 ? 
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_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             2012-11-09
_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            1
_cell_length_a                   19.907(2)
_cell_length_b                   7.7643(10)
_cell_length_c                   11.2139(14)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    100.02
_cell_measurement_theta_max      34.71
_cell_measurement_theta_min      2.82
_cell_volume                     1733.3(4)
_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.
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_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.02
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0718
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            94133
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         2.05
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.537
_exptl_absorpt_correction_T_max  0.809
_exptl_absorpt_correction_T_min  0.528
_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    3.053
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1488.2
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.949
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.194
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(6)
_refine_ls_extinction_coef       0.0012(2)
_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   1.033
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         6671
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+10.7856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1130
_reflns_number_gt                6355
_reflns_number_total             6671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402177j_si_003.cif
_cod_data_source_block           Compound_3
_cod_database_code               4337514
_olex2_refinement_description
;
1. Shared sites
{O1, F1}
{O3, F3}
{O4, F4}
{O5, F5}
{O6, F6}
{O7, F7}
{O8, F8}
{O10, F10}
{O11, F11}
{O12, F12}
{O15, F15}
2. Uiso/Uaniso restraints and constraints
Uanis(O1) = Uanis(F1)
Uanis(O3) = Uanis(F3)
Uanis(O4) = Uanis(F4)
Uanis(O5) = Uanis(F5)
Uanis(O6) = Uanis(F6)
Uanis(O7) = Uanis(F7)
Uanis(O8) = Uanis(F8)
Uanis(O10) = Uanis(F10)
Uanis(O11) = Uanis(F11)
Uanis(O12) = Uanis(F12)
Uanis(O15) = Uanis(F15)
Uanis(O2) = Uanis(F2)
Uanis(O13) = Uanis(F13)
3. Others
 Sof(K3A)=1-Sof(K3B)=Sof(Cl1)=1-Sof(K3B)
 Sof(K5A)=1-Sof(K5B)
 Fixed Sof: F1(0.75) F2(0.375) 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(0.375) O1(0.25) O2(0.125)
 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(0.125)
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