Polyoxometalate built-in conjugated microporous polymers for visible-light heterogeneous photocatalysis
Li, Yusen; Liu, Mingxuan; Chen, Long; Journal of Materials Chemistry A 5 (2017) 13757–; doi:10.1039/C7TA03776G

data_7236588
_publ_section_title
;
 Polyoxometalate built-in conjugated microporous polymers for
 visible-light heterogeneous photocatalysis
;
_journal_issue                   26
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              13757
_journal_paper_doi               10.1039/C7TA03776G
_journal_volume                  5
_journal_year                    2017
_chemical_formula_moiety
'C22 H20 Br4 Mn Mo6 N2 O26, 3(C16 H36 N), 2(C2 H3 N)'
_chemical_formula_sum            'C74 H134 Br4 Mn Mo6 N7 O26'
_chemical_formula_weight         2488.09
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_audit_update_record
;
2017-01-06 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 127.042(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.284(5)
_cell_length_b                   14.7645(18)
_cell_length_c                   24.392(4)
_cell_measurement_reflns_used    8062
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     9855(3)
_computing_cell_refinement
'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_detector                 PILT
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Xtalab p200'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41881
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.020
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_min         3.008
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Crystalclear
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5008
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   1.000
_exptl_transmission_factor_min   0.848
_refine_diff_density_max         1.181
_refine_diff_density_min         -2.594
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         8679
_refine_ls_number_restraints     271
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+229.6790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
_refine_ls_wR_factor_ref         0.1800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6393
_reflns_number_total             8679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ta03776g2.cif
_cod_data_source_block           shelx
_cod_database_code               7236588
_shelx_shelxl_version_number     2014/8
_shelx_estimated_absorpt_t_max   0.749
_shelx_estimated_absorpt_t_min   0.629
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-H1
 0.9 with sigma of 0.01
 C33-C34 = C33-C34' = C34-C35 = C34'-C35'
 1.54 with sigma of 0.01
 C12-C13 = C12-C13' = C13-C14 = C13'-C14' = C14-C15 = C14'-C15'
 1.54 with sigma of 0.01
 C28-C29 = C28-C29' = C29-C30 = C29'-C30' = C30-C31 = C30'-C31'
 1.54 with sigma of 0.01
 C29'-C31' = C29-C31
 2.52 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C34 \\sim C35 \\sim C34' \\sim C35': within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C13 \\sim C14 \\sim C15 \\sim C13' \\sim C14' \\sim C15': within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C29 \\sim C30 \\sim C31 \\sim C29' \\sim C30' \\sim C31': within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C34') \\sim Ueq, Uanis(C35')
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C13')
\\sim Ueq, Uanis(C14') \\sim Ueq, Uanis(C15') \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C29')
\\sim Ueq, Uanis(C30') \\sim Ueq, Uanis(C31') \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H12A(0.5) H12B(0.5) H12C(0.5) H12D(0.5) C13(0.5) H13A(0.5)
 H13B(0.5) C14(0.5) H14A(0.5) H14B(0.5) C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5)
 C13'(0.5) H13C(0.5) H13D(0.5) C14'(0.5) H14C(0.5) H14D(0.5) C15'(0.5)
 H15D(0.5) H15E(0.5) H15F(0.5) H22A(0.5) H22B(0.5) H22C(0.5) H22D(0.5) C23(0.5)
 H23A(0.5) H23B(0.5) H23C(0.5) C23'(0.5) H23D(0.5) H23E(0.5) H23F(0.5)
 H28A(0.5) H28B(0.5) H28C(0.5) H28D(0.5) C29(0.5) H29A(0.5) H29B(0.5) C30(0.5)
 H30A(0.5) H30B(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) C29'(0.5) H29C(0.5)
 H29D(0.5) C30'(0.5) H30C(0.5) H30D(0.5) C31'(0.5) H31D(0.5) H31E(0.5)
 H31F(0.5) H33A(0.5) H33B(0.5) H33C(0.5) H33D(0.5) C34(0.5) H34A(0.5) H34B(0.5)
 C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C34'(0.5) H34C(0.5) H34D(0.5) C35'(0.5)
 H35D(0.5) H35E(0.5) H35F(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C12(H12C,H12D),
 C13(H13A,H13B), C14(H14A,H14B), C13'(H13C,H13D), C14'(H14C,H14D), C16(H16A,
 H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C22(H22C,H22D), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
  C28(H28A,H28B), C28(H28C,H28D), C29(H29A,H29B), C30(H30A,H30B), C29'(H29C,
 H29D), C30'(H30C,H30D), C32(H32A,H32B), C33(H33A,H33B), C33(H33C,H33D),
 C34(H34A,H34B), C34'(H34C,H34D)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C15'(H15D,H15E,H15F), C19(H19A,H19B,H19C), C23(H23A,H23B,
 H23C), C23'(H23D,H23E,H23F), C27(H27A,H27B,H27C), C31(H31A,H31B,H31C),
 C31'(H31D,H31E,H31F), C35(H35A,H35B,H35C), C35'(H35D,H35E,H35F), C37(H37A,H37B,
 H37C)
;
_shelx_res_checksum              65253
_shelx_hkl_checksum              6586
_olex2_submission_special_instructions 'No special instructions were received'