Crystal growth of four oxovanadium(IV) tartrates prepared via a mild two-step hydrothermal method: observation of spin-dimer behavior and second harmonic generation.
Cortese, Anthony J.; Wilkins, Branford; Smith, Mark D.; Yeon, Jeongho; Morrison, Gregory; Tran, T. Thao; Halasyamani, P. Shiv; zur Loye, Hans-Conrad; Inorganic chemistry 54 (2015) 4011–4020; doi:10.1021/acs.inorgchem.5b00275

data_4346092
_publ_section_title
;
 Crystal growth of four oxovanadium(IV) tartrates prepared via a mild
 two-step hydrothermal method: observation of spin-dimer behavior and
 second harmonic generation.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4011
_journal_page_last               4020
_journal_paper_doi               10.1021/acs.inorgchem.5b00275
_journal_volume                  54
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C8 H6 K2 O14 V2, 3.95(H2 O)'
_chemical_formula_sum            'C8 H13.91 K2 O17.95 V2'
_chemical_formula_weight         577.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.4341(13)
_cell_length_b                   17.311(3)
_cell_length_c                   25.140(4)
_cell_measurement_reflns_used    2647
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.644
_cell_measurement_theta_min      2.353
_cell_volume                     3670.5(10)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.631 (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            20299
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.113
_diffrn_reflns_theta_min         1.620
_diffrn_source_current           37.0
_diffrn_source_power             1.739
_diffrn_source_voltage           47.0
_exptl_absorpt_coefficient_mu    1.566
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.090
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             2317
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 1153 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         3291
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0199P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0638
_reflns_Friedel_coverage         0.768
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2906
_reflns_number_total             3291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00275_si_002.cif
_cod_data_source_block           bw1041bm
_cod_database_code               4346092
_shelxl_version_number           2014-1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O3-H3A = O10-H10A
 0.84 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(K3A) = Uanis(K3B)
Uiso(O17D) = Uiso(O17E)
4. Others
 1*[Sof(O16A)]+1*[Sof(O16B)]+1*[Sof(O16C)]=1 with esd of 0.00001
 Sof(K3B)=0.5*(1-FVAR(2))
 Sof(K3A)=0.5*FVAR(2)
 Uiso(O1S)=Uiso(O2S)=Uiso(O3S)=Uiso(O4S)=FVAR(2)
 Sof(O15B)=1-FVAR(3)
 Sof(O15A)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7)
;
_shelx_res_checksum              4286
_shelx_hkl_checksum              20959
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'