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_7228073
_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         'As2 Mo6 O26, C42 H42 Cu N12, 2(H2 O)'
_chemical_formula_sum            'C42 H46 As2 Cu Mo6 N12 O28'
_chemical_formula_weight         1955.93
_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             2017-03-15
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.14 svn.r3398 for OlexSys, GUI svn.r5328)
;
_audit_update_record
;
2017-03-16 deposited with the CCDC.
2017-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                115.4950(10)
_cell_angle_beta                 100.7190(10)
_cell_angle_gamma                99.2610(10)
_cell_formula_units_Z            1
_cell_length_a                   10.8652(5)
_cell_length_b                   11.9690(6)
_cell_length_c                   13.1751(6)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.26
_cell_volume                     1462.36(12)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_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 0.985
_diffrn_measured_fraction_theta_max 0.956
_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  0.0130
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13138
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.348
_diffrn_reflns_theta_min         2.257
_exptl_absorpt_coefficient_mu    2.823
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0582 before and 0.0283 after correction. The Ratio of minimum to maximum transmission is 0.8541. The \l/2 correction factor is 0.00150.'
_exptl_crystal_density_diffrn    2.221
_exptl_crystal_description       block
_exptl_crystal_F_000             953
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.499
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6978
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0205P)^2^+4.6668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6630
_reflns_number_total             6978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00319f2.cif
_cod_data_source_block           111
_cod_database_code               7228073
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C18A-C18
 0.3 with sigma of 0.02
 C20-C21 \\sim C20A-C21A
 with sigma of 0.02
3. Rigid bond restraints
 N5, N5, N5, N5, N5, N5, N5, N6, N6, N6, N6, N6, C18, C18, C19, C19, C19, C20,
 C20, C20, C21, C21, C21, C19A, C19A, C19A, C20A, C20A, C20A, C21A, C21A, C21A,
 C18A, C18A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N5 \\sim N5 \\sim N5 \\sim N5 \\sim N5 \\sim N5 \\sim N5 \\sim N6 \\sim N6
\\sim N6 \\sim N6 \\sim N6 \\sim C18 \\sim C18 \\sim C19 \\sim C19 \\sim C19
\\sim C20 \\sim C20 \\sim C20 \\sim C21 \\sim C21 \\sim C21 \\sim C19A \\sim
C19A \\sim C19A \\sim C20A \\sim C20A \\sim C20A \\sim C21A \\sim C21A \\sim
C21A \\sim C18A \\sim C18A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
5. Others
 Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=
 Sof(C21A)=Sof(H21A)=1-FVAR(1)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=
 Sof(H21)=FVAR(1)
6.a Free rotating group:
 O14(H14A,H14B)
6.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C11(H11A,H11B), C18(H18A,H18B), C18A(H18C,H18D)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C16(H16), C17(H17), C19(H19), C19A(H19A), C20(H20), C20A(H20A),
 C21(H21), C21A(H21A)
;
_olex2_submission_special_instructions 'No special instructions were received'