Positional isomerism-driven two 3D pillar-layered metal-organic frameworks: Syntheses, topological structures and photoluminescence properties
Sun, Yayong; Zhao, Siwei; Ma, Haoran; Han, Yi; Liu, Kang; Wang, Lei; Journal of Solid State Chemistry 238 (2016) 284–290; doi:10.1016/j.jssc.2016.04.001

data_1561521
_publ_section_title
;
 Positional isomerism-driven two 3D pillar-layered metal-organic
 frameworks: Syntheses, topological structures and photoluminescence
 properties
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              284
_journal_page_last               290
_journal_paper_doi               10.1016/j.jssc.2016.04.001
_journal_volume                  238
_journal_year                    2016
_chemical_formula_moiety         '0.25(C304 H288 K8 N32 O144 Zn20)'
_chemical_formula_sum            'C76 H72 K2 N8 O36 Zn5'
_chemical_formula_weight         2078.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 104.732(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.7860(14)
_cell_length_b                   12.9841(2)
_cell_length_c                   16.5910(6)
_cell_measurement_reflns_used    13669
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.4630
_cell_measurement_theta_min      2.3850
_cell_volume                     7872.2(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.5095
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0059263000
_diffrn_orient_matrix_UB_12      -0.0417395000
_diffrn_orient_matrix_UB_13      -0.0020743000
_diffrn_orient_matrix_UB_21      -0.0042326000
_diffrn_orient_matrix_UB_22      0.0145475000
_diffrn_orient_matrix_UB_23      -0.0353512000
_diffrn_orient_matrix_UB_31      0.0575079000
_diffrn_orient_matrix_UB_32      0.0005471000
_diffrn_orient_matrix_UB_33      -0.0159034000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32305
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.175
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.710
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4240
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         6960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+9.0050P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0676
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5909
_reflns_number_total             6960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2016-238-284.cif
_cod_data_source_block           2
_cod_database_code               1561521
_chemical_oxdiff_formula         'C1 O1 N1 Zn1'
_reflns_odcompleteness_completeness 99.94
_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 C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Rotating group:
 O17(H17A,H17B)
2.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C27(H27A,H27B), C34(H34A,H34B), C10(H10A,H10B), C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
 C32(H32), C24(H24), C14(H14), C31(H31), C23(H23), C35(H35), C16(H16), C8(H8),
 C6(H6), C18(H18), C4(H4), C30(H30), C36(H36), C29(H29)
2.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              29646
_shelx_hkl_checksum              67060