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_1563791
_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         'C129 H100 N4 O33 Zn9'
_chemical_formula_sum            'C129 H100 N4 O33 Zn9'
_chemical_formula_weight         2822.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                101.858(2)
_cell_angle_beta                 93.315(2)
_cell_angle_gamma                109.524(2)
_cell_formula_units_Z            1
_cell_length_a                   12.4606(10)
_cell_length_b                   15.2889(12)
_cell_length_c                   20.6221(18)
_cell_measurement_reflns_used    2302
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      23.6
_cell_measurement_theta_min      2.2
_cell_volume                     3589.5(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.1005
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23062
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.021
_diffrn_reflns_theta_max         25.021
_diffrn_reflns_theta_min         1.455
_exptl_absorpt_coefficient_mu    1.544
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.120
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1034
_refine_ls_number_reflns         12611
_refine_ls_number_restraints     1153
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0708
_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^)+(0.1002P)^2^+7.5819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1935
_refine_ls_wR_factor_ref         0.2123
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8145
_reflns_number_total             12611
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           1
_cod_database_code               1563791
_shelx_estimated_absorpt_t_max   0.768
_shelx_estimated_absorpt_t_min   0.727
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H14-O14
 0.85 with sigma of 0.02
 C23A-C35A
 1.5 with sigma of 0.02
 O13-C57 = C57-O12
 1.2 with sigma of 0.02
 C23-C19 = C65-C61 = C14-C13
 1.5 with sigma of 0.02
 H14A-H23A_$2
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C67)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C50) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C51) \\sim Ueq,
Uanis(O12) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C70A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23A) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C65A)
\\sim Ueq, Uanis(C65) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. 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
5. Others
 Sof(O15B)=1-FVAR(1)
 Sof(O15A)=FVAR(1)
 Fixed Sof: O10(0.5) O11(0.5) O12(0.5) O13(0.5) C3(0.5) H3(0.5) C4(0.5)
 H4(0.5) C6(0.5) H6(0.5) C7(0.5) H7(0.5) H19(0.5) C23(0.5) H23A(0.5) H23B(0.5)
 H23C(0.5) C32(0.5) H32(0.5) C33(0.5) H33(0.5) C35(0.5) H35(0.5) C36(0.5)
 H36(0.5) C43(0.5) C44(0.5) C45(0.5) H45(0.5) C46(0.5) H46(0.5) C47(0.5)
 C48(0.5) C49(0.5) H49(0.5) C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5) C51(0.5)
 C52(0.5) H52(0.5) C53(0.5) H53(0.5) C54(0.5) C55(0.5) H55(0.5) C56(0.5)
 H56(0.5) C57(0.5) C60(0.5) H60(0.5) C61(0.5) C63(0.5) H63(0.5) C64(0.5)
 H64(0.5) C65(0.5) H65A(0.5) H65B(0.5) H65C(0.5) C67(0.5) H67(0.5) C68(0.5)
 H68(0.5) C70(0.5) H70(0.5) C71(0.5) H71(0.5) C67A(0.5) C68A(0.5) H68A(0.5)
 C71A(0.5) H71A(0.5) C70A(0.5) H70A(0.5) C60A(0.5) H60A(0.5) C61A(0.5)
 H61A(0.5) C63A(0.5) H63A(0.5) C64A(0.5) H64A(0.5) C65A(0.5) H65D(0.5)
 H65E(0.5) H65F(0.5) C35A(0.5) C36A(0.5) H36A(0.5) C32A(0.5) H32A(0.5)
 C33A(0.5) H33A(0.5) C23A(0.5) H23D(0.5) H23E(0.5) H23F(0.5) O19(0.5) H19A(0.5)
 H19B(0.5) C4A(0.5) H4A(0.5) C3A(0.5) H3A(0.5) C7A(0.5) H7A(0.5) C6A(0.5)
 H6A(0.5)
6.a Riding coordinates:
 O9(H9), O14(H14), C50(H50A,H50B,H50C), C23A(H23D,H23E,H23F), O19(H19A,H19B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9A), C10(H10), C12(H12), C18(H18),
 C19(H19), C21(H21), C22(H22), C24(H24), C25(H25), C28(H28), C32(H32), C33(H33),
  C35(H35), C36(H36), C37(H37), C40(H40), C41(H41), C45(H45), C46(H46),
 C49(H49), C52(H52), C53(H53), C55(H55), C56(H56), C60(H60), C63(H63), C64(H64),
  C67(H67), C68(H68), C70(H70), C71(H71), C68A(H68A), C71A(H71A), C70A(H70A),
 C60A(H60A), C61A(H61A), C63A(H63A), C64A(H64A), C36A(H36A), C32A(H32A),
 C33A(H33A), C4A(H4A), C3A(H3A), C7A(H7A), C6A(H6A)
6.c Fitted hexagon refined as free rotating group:
 C44(C45,C46,C47,C48,C49), C51(C52,C53,C54,C55,C56)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C29(H29A,H29B,H29C), C42(H42A,H42B,
 H42C), C65(H65A,H65B,H65C), C65A(H65D,H65E,H65F)
;
_shelx_res_checksum              56457
_shelx_hkl_checksum              53603
_shelx_fab_checksum              44546
_olex2_submission_special_instructions 'No special instructions were received'