A Gigantic Polyoxozirconate with Visible Photoactivity
Liu, Bo; Xu, Tingting; Hou, Xudong; Wang, Yang; Zhang, Jun; Zhang, Junxiang; Dalton Trans.  (2017) –; doi:10.1039/C7DT02013A

data_7043543
_publ_section_title
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 A Gigantic Polyoxozirconate with Visible Photoactivity
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02013A
_journal_year                    2017
_chemical_formula_moiety         'C196 H142 O79 Zr18'
_chemical_formula_sum            'C196 H142 O79 Zr18'
_chemical_formula_weight         5403.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-05-24
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-05-24 deposited with the CCDC.
2017-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.824(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.3272(9)
_cell_length_b                   20.6226(6)
_cell_length_c                   35.7721(11)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.11
_cell_measurement_theta_min      2.17
_cell_volume                     20789.5(11)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.976
_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  0.1525
_diffrn_reflns_av_unetI/netI     0.2119
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            149136
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         1.887
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_description       block
_exptl_crystal_F_000             10680
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_platon_squeeze_details          'TITL ab P 1 21/c 1 R = 0.07'
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2550
_refine_ls_number_reflns         46561
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.2101
_refine_ls_R_factor_gt           0.0713
_refine_ls_shift/su_max          0.112
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0803P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19811
_reflns_number_total             46561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02013a2.cif
_cod_data_source_block           ab
_cod_database_code               7043543
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.777
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 H53-O53
 1 with sigma of 0.02
 H52-O52
 1 with sigma of 0.02
 C80-C83
 1.4 with sigma of 0.02
 C141-C144
 1.4 with sigma of 0.02
 C33-C37
 1.4 with sigma of 0.02
 C32-C31
 1.5 with sigma of 0.01
 C37-C33
 1.5 with sigma of 0.01
 C88-C86
 1.5 with sigma of 0.01
 C149-C147
 1.45 with sigma of 0.01
 C66-C69
 1.5 with sigma of 0.01
3. Rigid bond restraints
 O34, C116
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C186, C187, C43, C45, C151, C152, C171, C172
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C84, C85
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C97, C99
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C48, C51
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C170, C168, C169, C195, C171, C172
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C96, C97
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C135, C139
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C179, C180
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C192, C193
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C90, C91
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C90 \\sim C92: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C187) \\sim Ueq, Uanis(C186) \\sim Ueq, Uanis(C185) \\sim Ueq,
Uanis(C183) \\sim Ueq, Uanis(C181) \\sim Ueq, Uanis(C184) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C172) \\sim Ueq, Uanis(C170) \\sim Ueq, Uanis(C168) \\sim Ueq,
Uanis(C169) \\sim Ueq, Uanis(C195) \\sim Ueq, Uanis(C171) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C183, C185, C186, C187, C184, C181
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C9(H9), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32),
  C28(H28), C29(H29), C30(H30), C31(H31), C34(H34), C36(H36), C35(H35),
 C38(H38), C37(H37), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C47(H47),
  C48(H48), C49(H49), C50(H50), C51(H51), C54(H54), C55(H55), C56(H56),
 C57(H57), C58(H58), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C68(H68),
  C70(H70), C72(H72), C71(H71), C69(H69), C74(H74), C76(H76), C77(H77),
 C78(H78), C79(H79), C81(H81), C82(H82), C83(H83), C84(H84), C85(H85), C89(H89),
  C92(H92), C90(H90), C91(H91), C88(H88), C95(H95), C96(H96), C97(H97),
 C98(H98), C99(H99), C101(H101), C103(H103), C104(H104), C105(H105), C106(H106),
  C108(H108), C110(H110), C111(H111), C112(H112), C113(H113), C115(H115),
 C117(H117), C118(H118), C120(H120), C122(H122), C123(H123), C124(H124),
 C127(H127), C128(H128), C129(H129), C134(H134), C135(H135), C136(H136),
 C137(H137), C138(H138), C139(H139), C144(H144), C142(H142), C194(H194),
 C145(H145), C143(H143), C149(H149), C152(H152), C151(H151), C150(H150),
 C148(H148), C153(H153), C154(H154), C155(H155), C156(H156), C157(H157),
 C158(H158), C159(H159), C160(H160), C161(H161), C164(H164), C165(H165),
 C172(H172), C170(H170), C169(H169), C195(H195), C171(H171), C174(H174),
 C175(H175), C177(H177), C178(H178), C179(H179), C180(H180), C183(H183),
 C185(H185), C186(H186), C187(H187), C184(H184), C188(H188), C189(H189),
 C190(H190), C191(H191), C192(H192), C193(H193), C196(H196)
6.b Fitted hexagon refined as free rotating group:
 C32(C28,C27,C29,C30,C31), C33(C34,C36,C35,C38,C37), C66(C68,C70,C72,C71,C69),
 C86(C89,C92,C90,C91,C88), C141(C144,C142,C194,C145,C143), C147(C149,C152,C151,
 C150,C148), C172(C170,C168,C169,C195,C171), C183(C185,C186,C187,C184,C181)
;
_olex2_submission_special_instructions 'No special instructions were received'