Octahedral Tilting in MM'X4 Metal-Oxide Organic Layer Structures
Marie Vougo-Zanda; Ekaterina V. Anokhina; Selma Duhovic; Lumei Liu; Xiqu Wang; Oluwakemi A. Oloba; Thomas A. Albright; Allan J. Jacobson; Inorganic Chemistry 47 (2008) 4746–4751; doi:10.1021/ic8000448

data_4304941
_publ_contact_author_address
; 
"Department of Chemistry, University of Houston, Houston, Texas 77204-5003"
;
_publ_contact_author_email       ajjacob@uh.edu
_publ_contact_author_fax         7137432787
_publ_contact_author_name        'Allan J. Jacobson'
_publ_contact_author_phone       7137432785
_publ_section_title
;
Octahedral Tilting in MM'X4 Metal-Oxide Organic Layer Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4746
_journal_page_last               4751
_journal_paper_doi               10.1021/ic8000448
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C4 H3.1 F0.3 O4.1 V'
_chemical_formula_weight         173.40
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           53
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2'
_symmetry_space_group_name_H-M   'P m n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.101(2)
_cell_length_b                   3.8416(11)
_cell_length_c                   20.570(6)
_cell_measurement_reflns_used    726
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     561.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  Bruker-ApexII
_diffrn_measurement_method       'narrow frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0192
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -2
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            3242
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_time  10h
_diffrn_standards_number         50frame
_exptl_absorpt_coefficient_mu    1.708
_exptl_absorpt_correction_T_max  0.7401
_exptl_absorpt_correction_T_min  0.5322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-ApexII
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.052
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             342
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.250
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         726
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.249
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0340P)^2^+1.0980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0912
_reflns_number_gt                691
_reflns_number_total             726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8000448-file002_1.cif
_cod_data_source_block           Compound1-V
_cod_original_formula_sum        'C4 H3.10 F0.30 O4.10 V'
_cod_database_code               4304941