A series of 0D to 3D Anderson-type polyoxometalate-based compounds obtained under ambient and hydrothermal conditions
Ying, Jun; Chen, Ya-Guang; Wang, Xiu-Yan; CrystEngComm 21 (2019) 1168–; doi:10.1039/C8CE01971A

data_7232072
_publ_section_title
;
 A series of 0D to 3D Anderson-type polyoxometalate-based compounds
 obtained under ambient and hydrothermal conditions
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1168
_journal_paper_doi               10.1039/C8CE01971A
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety
'C2 H13 Al Cu0.5 Mo6 N2 O24, C4 H18 Cu2 N4 O2, O'
_chemical_formula_sum            'C6 H31 Al Cu2.5 Mo6 N6 O27'
_chemical_formula_weight         1380.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-18 deposited with the CCDC.
2019-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                87.291(3)
_cell_angle_beta                 85.271(5)
_cell_angle_gamma                84.015(5)
_cell_formula_units_Z            1
_cell_length_a                   6.4672(16)
_cell_length_b                   10.482(3)
_cell_length_c                   13.154(3)
_cell_measurement_reflns_used    838
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.36
_cell_measurement_theta_min      2.55
_cell_volume                     883.1(4)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_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  0.0587
_diffrn_reflns_av_unetI/netI     0.1315
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5063
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.555
_exptl_absorpt_coefficient_mu    3.653
_exptl_absorpt_correction_T_max  0.674
_exptl_absorpt_correction_T_min  0.581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SABABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             662
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.509
_refine_diff_density_min         -1.233
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3095
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0537P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1289
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1810
_reflns_number_total             3095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01971a2.cif
_cod_data_source_block           y_CCDC4
_cod_depositor_comments
'Adding full bibliography for 7232067--7232073.cif.'
_cod_original_formula_sum        'C6 H31 Al Cu2.50 Mo6 N6 O27'
_cod_database_code               7232072
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All N(H,H,H,H) groups
2. Restrained distances
 H13-O13
 0.85 with sigma of 0.02
 H12-O12 = H11-O11 = H1-O1
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Cu3, N3, C4, C3, N4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: Cu3(0.25) N3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4(0.5) C3(0.5)
 H3C(0.5) H3D(0.5) N4(0.5) H4A(0.5) H4B(0.5) O1W(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), N1(H1C,H1D), N2(H2C,H2D), N3(H3A,H3B), C3(H3C,H3D),
 N4(H4A,H4B)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4)
;
_shelx_res_checksum              98004
_olex2_submission_special_instructions 'No special instructions were received'