The Role of Polar, Lamdba (Λ)-Shaped Building Units in Noncentrosymmetric Inorganic Structures
Martin D. Donakowski; Romain Gautier; Jeongho Yeon; Donald T. Moore; Juan C. Nino; P. Shiv Halasyamani; Kenneth R. Poeppelmeier; Journal of the American Chemical Society 134 (2012) 7679–7689; doi:10.1021/ja210984k

data_4117900
_publ_contact_author_address
;Department of Chemistry
Northwestern University
Evanston, Illinois 60208-3113
USA
;
_publ_contact_author_email       krp@northwestern.edu
_publ_contact_author_name        'Poeppelmeier, Kenneth'
_publ_contact_author_phone       '(708) 491-3505'
_publ_section_title
;
 The Role of Polar, Lamdba (\L)-Shaped Building Units in
 Noncentrosymmetric Inorganic Structures
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7679
_journal_page_last               7689
_journal_paper_doi               10.1021/ja210984k
_journal_volume                  134
_journal_year                    2012
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'Cu F4 H12 O7 V, H2 O'
_chemical_formula_sum            'Cu F4 H14 O8 V'
_chemical_formula_weight         332.59
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2011-06-07T15:38:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.63155(15)
_cell_length_b                   8.22032(8)
_cell_length_c                   7.36600(7)
_cell_measurement_reflns_used    9630
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.2818
_cell_measurement_theta_min      2.7652
_cell_measurement_wavelength     0.71073
_cell_volume                     946.504(16)
_computing_cell_refinement       'SAINT V7.68A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_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    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_type       'x-axis to radiation source'
_diffrn_orient_matrix_UB_11      -0.02288
_diffrn_orient_matrix_UB_12      -0.723942E-1
_diffrn_orient_matrix_UB_13      -0.502688E-1
_diffrn_orient_matrix_UB_21      0.130816
_diffrn_orient_matrix_UB_22      -0.325225E-1
_diffrn_orient_matrix_UB_23      -0.268679E-3
_diffrn_orient_matrix_UB_31      -0.281801E-1
_diffrn_orient_matrix_UB_32      -0.921957E-1
_diffrn_orient_matrix_UB_33      0.39567E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            27775
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        30.33
_diffrn_reflns_theta_max         30.33
_diffrn_reflns_theta_min         2.61
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    3.319
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.334
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.214
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.024(6)
_refine_ls_extinction_coef       0.0136(4)
_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   1.101
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2806
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0124
_refine_ls_R_factor_gt           0.012
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+0.1164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0329
_refine_ls_wR_factor_ref         0.0339
_reflns_number_gt                2754
_reflns_number_total             2806
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210984k_si_004.cif
_cod_data_source_block           n0750_0m
_cod_original_sg_symbol_Hall     'P 2c -2n '
_cod_database_code               4117900