Three novel and various isopolymolybdate-based hybrids built from the carboxyl oxygen atoms of in situ ligands: substituent-tuned assembly, architectures and properties.
Wang, Xiu-Li; Zhang, Rui; Wang, Xiang; Lin, Hong-Yan; Liu, Guo-Cheng; Zhang, Hui-Xiu; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1965–1974; doi:10.1039/c6dt04185j

data_7041620
_publ_section_title
;
 Three novel and various isopolymolybdate-based hybrids built from the
 carboxyl oxygen atoms of in situ ligands: substituent-tuned assembly,
 architectures and properties.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1965
_journal_page_last               1974
_journal_paper_doi               10.1039/c6dt04185j
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C26 H20 Cu2 Mo8 N8 O31, 2(H2 O)'
_chemical_formula_sum            'C26 H23 Cu2 Mo8 N8 O33'
_chemical_formula_weight         1871.15
_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             2016-12-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2016-12-20 deposited with the CCDC.
2017-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                95.609(3)
_cell_angle_beta                 94.212(3)
_cell_angle_gamma                104.471(4)
_cell_formula_units_Z            2
_cell_length_a                   11.726(2)
_cell_length_b                   14.152(2)
_cell_length_c                   14.759(2)
_cell_measurement_reflns_used    2904
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      2.389
_cell_volume                     2347.9(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.1167
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16580
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.397
_diffrn_reflns_theta_min         1.394
_exptl_absorpt_coefficient_mu    3.058
_exptl_absorpt_correction_T_max  0.632
_exptl_absorpt_correction_T_min  0.565
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.645
_exptl_crystal_description       block
_exptl_crystal_F_000             1786
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.452
_refine_diff_density_min         -2.714
_refine_diff_density_rms         0.289
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         11634
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0683
_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^)+(0.0868P)^2^+0.0760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7476
_reflns_number_total             11634
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04185j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7041618--7041620.cif.'
_cod_database_code               7041620
_shelx_estimated_absorpt_t_max   0.657
_shelx_estimated_absorpt_t_min   0.594
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid bond restraints
 C2, C3, C6, C11, C21, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C5, C7, C13, C17, C19, C20, O25, O28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4, N4, N5, C16, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C2 \\sim C21 \\sim C3 \\sim C11 \\sim C6 \\sim C25: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C1 \\sim C5 \\sim C7 \\sim C13 \\sim C17 \\sim C19 \\sim C20 \\sim O25 \\sim
O28: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
N4 \\sim C4 \\sim C26 \\sim N5 \\sim C16: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(Cu1) = Uanis(Cu1A)
Uanis(O27A) = Uanis(O27)
4. Others
 Fixed Sof: Cu1(0.5) Cu1A(0.5) O27A(0.5) O27(0.5)
5.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C26(H26), C27(H27), C28(H28),
  C29(H29)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'