Unprecedented chi isomers of single-side triol-functionalized Anderson polyoxometalates and their proton-controlled isomer transformation
Jiangwei Zhang; Zhenhua Liu; Yichao Huang; Jin zhang; Jian Hao; Yongge Wei; Chem.Commun. 51 (2015) 9097–; doi:10.1039/C5cc02947C

data_7117206
_publ_section_title
;
 Unprecedented chi isomers of single-side triol-functionalized Anderson
 polyoxometalates and their proton-controlled isomer transformation
;
_journal_name_full               Chem.Commun.
_journal_page_first              9097
_journal_paper_doi               10.1039/C5cc02947C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'Cr H7 Mo6 O24, 6(H2 O), 2(C4 H12 N)'
_chemical_formula_sum            'C8 H43 Cr Mo6 N2 O30'
_chemical_formula_weight         1275.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/cc146zlx
_audit_creation_date             2015-03-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-25 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.122(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0834(3)
_cell_length_b                   11.5341(4)
_cell_length_c                   23.0245(6)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.999
_cell_measurement_theta_min      3.043
_cell_volume                     3965.47(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20239
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.043
_exptl_absorpt_coefficient_mu    2.190
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_correction_T_min  0.769
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2484
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         7784
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1567P)^2^+459.1487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1263
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6714
_reflns_number_total             7784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc02947c2.cif
_cod_data_source_block           compound6
_cod_original_cell_volume        3965.45(19)
_cod_database_code               7117206
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H6-H25B
 -2.2 with sigma of 0.01
 O28-H28A = O28-H28B = O25_$1-H25A_$1 = O25_$1-H25B_$1 = O29_$1-H29A_$1 =
 O29_$1-H29B_$1
 0.84 with sigma of 0.02
 O26-H26A = O26-H26B = O27_$3-H27A_$3 = O27_$3-H27B_$3
 0.84 with sigma of 0.02
 O28-H28A = O25_$1-H25B_$1
 0.82 with sigma of 0.02
 O9-H9
 0.9 with sigma of 0.02
 H6-H25A
 2 with sigma of 0.01
 H6-H30A
 2 with sigma of 0.01
 Mo3-H9
 2.2 with sigma of 0.01
 H28A-H28B = H25A_$1-H25B_$1 = H29A_$1-H29B_$1 = H26A_$1-H26B_$1 = H27A_$2-
 H27B_$2
 1.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Free rotating group:
 O30(H30A,H30B)
4.b Ternary CH refined with riding coordinates:
 O1(H1), O2(H2), O3(H3), O4(H4), O5(H5), O6(H6)
4.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C3(H3A,
 H3B,H3C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C1(H1A,H1B,H1C)
;