Assembly of Six [HxAs2Mo6O26](6-x)- Clusters-Based Hybrid Materials from 1D Chain to 3D Framework with Multiple Cu-N Complexes
Cong, Bowen; Su, Zhanhua; Zhao, Zhifeng; yu, baoyi; Zhao, Wenqi; Xia, Lin; ma, xiujuan; Zhou, Baibin; CrystEngComm  (2017) –; doi:10.1039/C7CE00319F

data_7228075
_publ_section_title
;
 Assembly of Six [HxAs2Mo6O26](6-x)- Clusters-Based Hybrid Materials from
 1D Chain to 3D Framework with Multiple Cu-N Complexes
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00319F
_journal_year                    2017
_chemical_formula_moiety         'C30 H30 As2 Cl Cu3 Mo6 N20 O26, H2 O'
_chemical_formula_sum            'C30 H32 As2 Cl Cu3 Mo6 N20 O27'
_chemical_formula_weight         2056.30
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-03-16 deposited with the CCDC.
2017-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                109.0810(10)
_cell_angle_beta                 103.5610(10)
_cell_angle_gamma                109.2280(10)
_cell_formula_units_Z            1
_cell_length_a                   11.0544(9)
_cell_length_b                   11.9897(10)
_cell_length_c                   12.6353(10)
_cell_measurement_reflns_used    6865
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.81
_cell_volume                     1380.2(2)
_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 0.983
_diffrn_measured_fraction_theta_max 0.952
_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  0.0163
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11092
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.337
_diffrn_reflns_theta_min         2.808
_exptl_absorpt_coefficient_mu    3.789
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1000 before and 0.0284 after correction. The Ratio of minimum to maximum transmission is 0.6665. The \l/2 correction factor is 0.00150.'
_exptl_crystal_density_diffrn    2.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             990
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         6553
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0212P)^2^+2.7240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5770
_reflns_number_total             6553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00319f2.cif
_cod_data_source_block           zw1404_0m
_cod_database_code               7228075
_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
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O5-As1A \\sim As1-O5A
 with sigma of 0.02
3. Rigid bond restraints
 Cl1, Cl1, N12, N12, N12, N9, N9, N9, N9, C16, C16, C16, C16, C17, C17, C17,
 C18, C18, C18, Cu2, Cu2, Cu2, Cu2, N11, N11, N11, C15, C15, C15, N10, N10, N10,
  N10, C14, C14, C14, C13, C13, C13, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl1 \\sim N12 \\sim N12 \\sim N12 \\sim N9 \\sim N9 \\sim N9 \\sim N9
\\sim C16 \\sim C16 \\sim C16 \\sim C16 \\sim C17 \\sim C17 \\sim C17 \\sim C18
\\sim C18 \\sim C18 \\sim Cu2 \\sim Cu2 \\sim Cu2 \\sim Cu2 \\sim N11 \\sim N11
\\sim N11 \\sim C15 \\sim C15 \\sim C15 \\sim N10 \\sim N10 \\sim N10 \\sim N10
\\sim C14 \\sim C14 \\sim C14 \\sim C14 \\sim C13 \\sim C13 \\sim C13 \\sim C13
\\sim C13: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
As1A \\sim O5: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(As1A) = Uanis(As1)
5. Others
 Sof(As1A)=Sof(O5)=1-FVAR(1)
 Sof(As1)=Sof(O5A)=FVAR(1)
 Fixed Sof: Cu2(0.5) Cl1(0.5) N9(0.5) N10(0.5) N11(0.5) H11(0.5) N12(0.5)
 H12(0.5) C13(0.5) C14(0.5) H14(0.5) C15(0.5) H15(0.5) C16(0.5) C17(0.5)
 H17(0.5) C18(0.5) H18(0.5) O14(0.5) H14A(0.5) H14B(0.5)
6.a Free rotating group:
 O14(H14A,H14B)
6.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), N7(H7), N8(H8), N11(H11), N12(H12), C2(H2), C3(H3), C5(H5A),
 C6(H6A), C8(H8A), C9(H9), C11(H11A), C12(H12A), C14(H14), C15(H15), C17(H17),
 C18(H18)
;
_olex2_submission_special_instructions 'No special instructions were received'