A helical chain-like organic-inorganic hybrid arsenotungstate with color-tunable photoluminescence.
Wu, Hechen; Wan, Rong; Si, Yanan; Ma, Pengtao; Wang, Jingping; Niu, Jingyang; Dalton transactions (Cambridge, England : 2003) 47 (2018) 1958–1965; doi:10.1039/c7dt04608a

data_7045205
_publ_section_title
;
 A helical chain-like organic-inorganic hybrid arsenotungstate with
 color-tunable photoluminescence.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1958
_journal_page_last               1965
_journal_paper_doi               10.1039/c7dt04608a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'0.25(C32 H104 As8 Na16 O368 Pr8 W84), 6(H4 O2)'
_chemical_formula_sum            'C8 H50 As2 Na4 O104 Pr2 W21'
_chemical_formula_weight         6194.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-31 deposited with the CCDC.
2018-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.160(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.802(5)
_cell_length_b                   28.389(8)
_cell_length_c                   21.365(9)
_cell_measurement_reflns_used    6401
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.61
_cell_measurement_theta_min      2.47
_cell_volume                     11345(6)
_computing_cell_refinement       'SAINT V8.18C'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.18C'
_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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29203
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         2.178
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.734
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1517 before and 0.0492 after correction.
The Ratio of minimum to maximum transmission is 0.4353.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.627
_exptl_crystal_description       block
_exptl_crystal_F_000             10848
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.663
_refine_diff_density_min         -2.685
_refine_diff_density_rms         0.293
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         10079
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+229.5643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1248
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7356
_reflns_number_total             10079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04608a2.cif
_cod_data_source_block           1588091
_cod_depositor_comments          'Adding full bibliography for 7045205.cif.'
_cod_database_code               7045205
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.122
_shelx_estimated_absorpt_t_min   0.078
_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
 C2-C3
 1.5 with sigma of 0.01
 O1W-H1WA = O1W-H1WB
 0.83 with sigma of 0.01
 O2W-H2WA = O2W-H2WB
 0.83 with sigma of 0.01
 O3W-H3WA = O3W-H3WB
 0.83 with sigma of 0.01
 O4W-H4WA = O4W-H4WB
 0.83 with sigma of 0.01
 O5W-H5WA = O5W-H5WB
 0.83 with sigma of 0.01
 O6W-H6WA = O6W-H6WB
 0.83 with sigma of 0.01
 O7W-H7WA = O7W-H7WB
 0.83 with sigma of 0.01
 O8W-H8WA = O8W-H8WB
 0.83 with sigma of 0.01
 O9W-H9WA = O9W-H9WB
 0.83 with sigma of 0.01
 O12W-H12A = O12W-H12B
 0.83 with sigma of 0.01
 H1WA-H1WB
 1.37 with sigma of 0.02
 H2WA-H2WB
 1.37 with sigma of 0.02
 H3WA-H3WB
 1.37 with sigma of 0.02
 H4WA-H4WB
 1.37 with sigma of 0.02
 H5WA-H5WB
 1.37 with sigma of 0.02
 H6WA-H6WB
 1.37 with sigma of 0.02
 H7WA-H7WB
 1.37 with sigma of 0.02
 H8WA-H8WB
 1.37 with sigma of 0.02
 H9WA-H9WB
 1.37 with sigma of 0.02
 H12A-H12B
 1.37 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C3 \\sim C2 \\sim C4: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O38) \\sim Ueq, Uanis(O41) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O4W) \\sim Ueq, Uanis(O8W) \\sim Ueq, Uanis(O9W) \\sim Ueq, Uanis(O10W)
\\sim Ueq, Uanis(O11W) \\sim Ueq, Uanis(O12W) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H3WA(0.5) H3WB(0.5) H8WA(0.5) H8WB(0.5)
5.a :
 O5W(H5WA,H5WB,O6W,H6WA,H6WB,O7W,H7WA,H7WB,O8W,H8WA,H8WB,O9W,H9WA,H9WB,O10W,
 H10A,H10B,O11W,H11A,H11B)
5.b Ternary CH refined with riding coordinates:
 C2(H2)
5.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
;
_shelx_res_checksum              75478
_shelx_fab_checksum              35967
_olex2_submission_special_instructions 'No special instructions were received'