Syntheses, structures, luminescent and catalytic properties of two 3D metal-organic frameworks
Xiao, Jun-Xia; Ma, De-Yun; Inorganica Chimica Acta 483 (2018) 6–11; doi:10.1016/j.ica.2018.07.054

data_1563792
_publ_section_title
;
 Syntheses, structures, luminescent and catalytic properties of two 3D
 metal-organic frameworks
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              6
_journal_page_last               11
_journal_paper_doi               10.1016/j.ica.2018.07.054
_journal_volume                  483
_journal_year                    2018
_chemical_formula_moiety         'C105 H72 O33 Pb11'
_chemical_formula_sum            'C105 H72 O33 Pb11'
_chemical_formula_weight         4140.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   26.6681(12)
_cell_length_b                   31.3068(13)
_cell_length_c                   56.946(2)
_cell_measurement_reflns_used    4717
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.60
_cell_measurement_theta_min      2.46
_cell_volume                     47544(3)
_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(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1366
_diffrn_reflns_av_unetI/netI     0.0780
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            75731
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.121
_diffrn_reflns_theta_max         25.121
_diffrn_reflns_theta_min         1.065
_exptl_absorpt_coefficient_mu    15.589
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.314
_exptl_crystal_description       block
_exptl_crystal_F_000             29879
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.127
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.246
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         10594
_refine_ls_number_restraints     950
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0382P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7538
_reflns_number_total             10594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               1563792
_shelx_estimated_absorpt_t_max   0.166
_shelx_estimated_absorpt_t_min   0.131
_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 C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C45A-C43A
 1.4 with sigma of 0.02
 C45-C43
 1.4 with sigma of 0.02
 C28-C29
 1.4 with sigma of 0.02
 C29-C24
 1.4 with sigma of 0.02
 C29-C28
 1.4 with sigma of 0.02
 C28-C27
 1.4 with sigma of 0.02
 C47-C52
 1.4 with sigma of 0.02
 C52-C51
 1.4 with sigma of 0.02
 C51-C50
 1.4 with sigma of 0.02
 C53A-C51A
 1.4 with sigma of 0.02
 C15-C6
 1.4 with sigma of 0.02
 H28-H30A
 2.2 with sigma of 0.02
 H28-H30B
 2.2 with sigma of 0.02
3. Restrained planarity
 C50A, C51A, C52A, C53A
 with sigma of 0.1
 C51, C50, C52, C49, C48, C47
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C45) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C45A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C15A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C52A) \\sim Ueq, Uanis(C51A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C53A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H41A)=Sof(C42)=Sof(C43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45A)=Sof(H45B)=
 Sof(H45C)=1-FVAR(1)
 Sof(H41)=Sof(C42A)=Sof(C43A)=Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(H45D)=
 Sof(H45E)=Sof(H45F)=FVAR(1)
 Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=1-FVAR(2)
 Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=FVAR(2)
 Fixed Sof: H6(0.5) H13(0.5) C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5) C15A(0.5)
 H15D(0.5) H15E(0.5) H15F(0.5) H49(0.5) H49A(0.5) C50(0.5) C50A(0.5) C51(0.5)
 H51(0.5) C51A(0.5) C52(0.5) H52(0.5) C52A(0.5) H52A(0.5) C53A(0.5) H53A(0.5)
 H53B(0.5) H53C(0.5)
7.a Riding coordinates:
 O2(H2)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C18(H18), C19(H19), C22(H22), C25(H25), C26(H26), C28(H28), C28A(H28A),
 C29(H29), C29A(H29A), C33(H33), C34(H34), C36(H36), C37(H37), C40(H40),
 C41(H41A), C41(H41), C44(H44), C44A(H44A), C48(H48), C49(H49), C49(H49A),
 C51(H51), C52(H52), C52A(H52A)
7.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C15A(H15D,H15E,H15F), C30(H30A,H30B,H30C), C45(H45A,H45B,
 H45C), C45A(H45D,H45E,H45F), C53A(H53A,H53B,H53C)
;
_shelx_res_checksum              19370
_shelx_hkl_checksum              27316
_shelx_fab_checksum              95292
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'