Three luminescent metal‒organic frameworks constructed from trinuclear zinc(ii) clusters and furan-2,5-dicarboxylate
Li, Huan-Huan; Niu, Zheng; Chen, Long; Jiang, Hao-Bin; Wang, Ya-Ping; Cheng, Peng; CrystEngComm 17 (2015) 5101–; doi:10.1039/C5CE00931F

data_1520081
_publ_section_title
;
 Three luminescent metal--organic frameworks constructed from trinuclear
 zinc(ii) clusters and furan-2,5-dicarboxylate
;
_journal_issue                   27
_journal_name_full               CrystEngComm
_journal_page_first              5101
_journal_paper_doi               10.1039/C5CE00931F
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C12 H4 O10 Zn1.5, C3 H7 N O, 1(C2 H8 N1)'
_chemical_formula_sum            'C17 H19 N2 O11 Zn1.5'
_chemical_formula_weight         525.40
_chemical_name_systematic
;
 ?
;
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2014-11-28 deposited with the CCDC.
2015-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.599(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3468(12)
_cell_length_b                   15.2267(8)
_cell_length_c                   17.6517(8)
_cell_measurement_reflns_used    4154
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      29.2245
_cell_measurement_theta_min      2.3815
_cell_volume                     2500.2(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.845
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0538116000
_diffrn_orient_matrix_UB_12      -0.0301480000
_diffrn_orient_matrix_UB_13      -0.0145539000
_diffrn_orient_matrix_UB_21      0.0463655000
_diffrn_orient_matrix_UB_22      -0.0355718000
_diffrn_orient_matrix_UB_23      0.0114783000
_diffrn_orient_matrix_UB_31      -0.0282249000
_diffrn_orient_matrix_UB_32      -0.0008232000
_diffrn_orient_matrix_UB_33      0.0359475000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11341
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.256
_diffrn_reflns_theta_min         2.566
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.503
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.005
_refine_diff_density_min         -2.540
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5754
_refine_ls_number_restraints     288
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0875
_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^)+(0.1330P)^2^+12.3200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2335
_refine_ls_wR_factor_ref         0.2587
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4215
_reflns_number_total             5754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00931f2.cif
_cod_data_source_block           p101209l2
_cod_depositor_comments
'Adding full bibliography for 1520079--1520081.cif.'
_cod_original_formula_sum        'C17 H19 N2 O11 Zn1.50'
_cod_database_code               1520081
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         C12ZN1
_chemical_oxdiff_usercomment     2010120138
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O12 \\sim C17 \\sim N2 \\sim C18 \\sim C16 \\sim N1 \\sim C14 \\sim O11 \\sim
C13 \\sim C15 \\sim C20' \\sim C19 \\sim N3' \\sim N3 \\sim C20 \\sim C19':
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O12) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(O11) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C20')
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(N3') \\sim Ueq, Uanis(N3) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C19') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(O2) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(O6)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq,
Uanis(O10) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Sof(N3')=Sof(H3'A)=Sof(H3'B)=Sof(C19')=Sof(H19D)=Sof(H19E)=Sof(H19F)=
 Sof(C20')=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(N3)=Sof(H3A)=Sof(H3B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=
 Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
 Fixed Sof: O11(0.5) N1(0.5) C13(0.5) H13(0.5) C14(0.5) H14A(0.5) H14B(0.5)
 H14C(0.5) C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5) O12(0.5) N2(0.5) C16(0.5)
 H16(0.5) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C18(0.5) H18A(0.5) H18B(0.5)
 H18C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N3'(H3'A,H3'B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C10(H10), C13(H13), C16(H16)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C19'(H19D,H19E,H19F),
 C20'(H20D,H20E,H20F)
;