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_1520080
_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
'C48 H16 O40 Zn6, 4(C2 H8 N), 3(C3 H7 N O), 1.17(O)'
_chemical_formula_sum            'C65 H69 N7 O44.17 Zn6'
_chemical_formula_weight         2047.15
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-28
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.10.28 svn.r3060 for OlexSys, GUI svn.r4951)
;
_audit_update_record
;
2014-11-28 deposited with the CCDC.
2015-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                85.110(4)
_cell_angle_beta                 65.988(5)
_cell_angle_gamma                89.663(4)
_cell_formula_units_Z            1
_cell_length_a                   12.6947(8)
_cell_length_b                   12.8242(6)
_cell_length_c                   14.7971(7)
_cell_measurement_reflns_used    7261
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      28.9944
_cell_measurement_theta_min      2.3314
_cell_volume                     2191.4(2)
_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 0.970
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -5.00   86.00   1.0000    2.7000
omega____ theta____ kappa____ phi______ frames
    -       18.1935   37.0000 -150.0000 91

  2 omega  -33.00   11.00   1.0000    2.7000
omega____ theta____ kappa____ phi______ frames
    -       18.1935  -77.0000  -60.0000 44

  3 omega   27.00   90.00   1.0000    2.7000
omega____ theta____ kappa____ phi______ frames
    -       18.1935 -150.0000  -45.0000 63

  4 omega   -3.00   55.00   1.0000    2.7000
omega____ theta____ kappa____ phi______ frames
    -       18.1935   77.0000    0.0000 58

  5 omega  -52.00   44.00   1.0000    2.7000
omega____ theta____ kappa____ phi______ frames
    -       18.1935  -37.0000   30.0000 96

  6 omega  -71.00  -45.00   1.0000    2.7000
omega____ theta____ kappa____ phi______ frames
    -      -18.8185  122.0000   63.0000 26
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0031795000
_diffrn_orient_matrix_UB_12      0.0048478000
_diffrn_orient_matrix_UB_13      0.0484269000
_diffrn_orient_matrix_UB_21      0.0603235000
_diffrn_orient_matrix_UB_22      0.0109213000
_diffrn_orient_matrix_UB_23      -0.0201829000
_diffrn_orient_matrix_UB_31      -0.0098728000
_diffrn_orient_matrix_UB_32      0.0542675000
_diffrn_orient_matrix_UB_33      -0.0052264000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_laue_measured_fraction_full 0.970
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14590
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         2.335
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.712
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87766
_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_density_diffrn    1.551
_exptl_crystal_description       strip
_exptl_crystal_F_000             1041
_refine_diff_density_max         1.819
_refine_diff_density_min         -1.970
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         7711
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0814P)^2^+9.0732P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6316
_reflns_number_total             7711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00931f2.cif
_cod_data_source_block           p101209j2
_cod_depositor_comments
'Adding full bibliography for 1520079--1520081.cif.'
_cod_database_code               1520080
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C12ZN1
_chemical_oxdiff_usercomment     2010120158
_reflns_odcompleteness_completeness 99.89
_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. Restrained distances
 C1A-C14
 2.5 with sigma of 0.02
 C11-N15
 1.5 with sigma of 0.02
 N15-C18
 1.5 with sigma of 0.02
 C1A-N12
 1.5 with sigma of 0.02
 N12-C14
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C14) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.0005
Uanis(C14) = Uanis(C18)
Uanis(C1A) = Uanis(C11)
Uanis(N12) = Uanis(N15)
Uanis(O13) = Uanis(C10) = Uanis(N9) = Uanis(C19) = Uanis(C17)
Uanis(O1) = Uanis(O2)
Uanis(O8BA) = Uanis(C6DA) = Uanis(O7BA)
4. Others
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(N15)=Sof(H15A)=Sof(H15B)=Sof(C18)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=1-FVAR(1)
 Sof(N12)=Sof(H12A)=Sof(H12B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C1A)=
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=FVAR(1)
 Fixed Sof: N9(0.5) C10(0.5) H10(0.5) O13(0.5) C17(0.5) H17A(0.5) H17B(0.5)
 H17C(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) O1(0.33333) O2(0.25)
5.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N12(H12A,H12B), N15(H15A,H15B)
5.b Aromatic/amide H refined with riding coordinates:
 C3CA(H3CA), C2DA(H2DA), C3DA(H3DA), C4DA(H4DA), C5DA(H5DA), C4EA(H4EA),
 C7EA(H7EA), C8EA(H8EA), C5(H5), C10(H10)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C11(H11A,
 H11B,H11C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              85360
_olex2_submission_special_instructions 'No special instructions were received'