Two unusual 3D honeycomb networks based on Wells–Dawson arsenomolybdates with d10 transition-metal-pyrazole connectors
Cong, Bo-Wen; Su, Zhan-Hua; Zhao, Zhi-Feng; Yu, Bao-Yi; Zhao, Wen-Qi; Ma, Xiu-Juan; Dalton Trans.  (2017) –; doi:10.1039/C7DT01240C

data_7043203
_publ_section_title
;
 Two unusual 3D honeycomb networks based on Wells--Dawson arsenomolybdates
 with d10 transition-metal-pyrazole connectors
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01240C
_journal_year                    2017
_chemical_formula_moiety         '0.5(As2 Mo18 O62), 3(C6 H8 Cu N4)'
_chemical_formula_sum            'C18 H24 As Cu3 Mo9 N12 O31'
_chemical_formula_weight         2033.49
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-20
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.14 svn.r3398 for OlexSys, GUI svn.r5328)
;
_audit_update_record
;
2017-03-27 deposited with the CCDC.
2017-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   22.1967(8)
_cell_length_b                   22.1967(8)
_cell_length_c                   34.780(3)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.01
_cell_measurement_theta_min      2.42
_cell_volume                     14840.1(15)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_collection       'Bruker SMART'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            40949
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.289
_diffrn_reflns_theta_min         2.541
_exptl_absorpt_coefficient_mu    4.223
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    2.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11544
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.306
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4088
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0228P)^2^+303.8790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3053
_reflns_number_total             4088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01240c2.cif
_cod_data_source_block           cbw6207_0m
_cod_original_cell_volume        14840.1(19)
_cod_database_code               7043203
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 N1-C1 \\sim C2-C3 \\sim C1-C2
 with sigma of 0.001
3. Rigid bond restraints
 N3, N4, C4, C6, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, N2, C1, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N3 \\sim N4 \\sim C4 \\sim C6 \\sim C5: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.01
N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.01
5. Others
 Fixed Sof: O9(0.5) O9A(0.5) O10(0.5) O10A(0.5) O11(0.5) O11A(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C1(H1), C2(H2A), C3(H3), N4(H4), C4(H4A), C5(H5), C6(H6)
;
_shelx_res_checksum              815
_shelx_fab_checksum              81103
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'