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_7228072
_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         'C40 H66 As2 Cu2 Mo6 N24 O26, O'
_chemical_formula_sum            'C40 H66 As2 Cu2 Mo6 N24 O27'
_chemical_formula_weight         2167.73
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-11
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-04-06 deposited with the CCDC.
2017-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                99.7490(10)
_cell_angle_beta                 105.5370(10)
_cell_angle_gamma                111.8780(10)
_cell_formula_units_Z            1
_cell_length_a                   12.5599(15)
_cell_length_b                   12.7481(15)
_cell_length_c                   13.3670(16)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.42
_cell_measurement_theta_min      2.64
_cell_volume                     1824.8(4)
_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 0.980
_diffrn_measured_fraction_theta_max 0.959
_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  0.0328
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16487
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.419
_diffrn_reflns_theta_min         2.644
_exptl_absorpt_coefficient_mu    2.556
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1021 before and 0.0473 after correction. The Ratio of minimum to maximum transmission is 0.4955. The \l/2 correction factor is 0.00150.'
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.597
_refine_diff_density_min         -1.752
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         8785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0498P)^2^+4.2777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8084
_reflns_number_total             8785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00319f2.cif
_cod_data_source_block           zwq102_0m
_cod_database_code               7228072
_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
2. Others
 Fixed Sof: O14(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3A,H3B), C4(H4A,H4B), C20(H20A,H20B), C19(H19A,H19B),
 C18(H18A,H18B), C9(H9A,H9B), C8(H8A,H8B), C11(H11A,H11B), C10(H10A,H10B),
 C12(H12A,H12B), C13(H13A,H13B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C16(H16), C15(H15), C14(H14), C7(H7), C6(H6), C2(H2), C17(H17)
;
_olex2_submission_special_instructions 'No special instructions were received'