Tuning Two-Dimensional Layer to Three-Dimensional Pillar-Layered Metal‒Organic Frameworks: Polycatenation and Interpenetration Behaviors
Chen, Di-ming; Zhang, Xiao-ping; Shi, Wei; Cheng, Peng; Crystal Growth & Design 14 (2014) 6261–; doi:10.1021/cg500942g

data_4512213
_publ_section_title
;
 Tuning Two-Dimensional Layer to Three-Dimensional Pillar-Layered
 Metal--Organic Frameworks: Polycatenation and Interpenetration Behaviors
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              6261
_journal_paper_doi               10.1021/cg500942g
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C48 H32 N4 O10 Zn2, O, 3(C4 H9 N O)'
_chemical_formula_sum            'C60 H59 N7 O14 Zn2'
_chemical_formula_weight         1232.88
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                88.492(5)
_cell_angle_beta                 87.735(4)
_cell_angle_gamma                89.118(6)
_cell_formula_units_Z            2
_cell_length_a                   7.4379(5)
_cell_length_b                   14.7017(12)
_cell_length_c                   25.1694(10)
_cell_measurement_reflns_used    5273
_cell_measurement_temperature    133(4)
_cell_measurement_theta_max      29.0230
_cell_measurement_theta_min      3.2360
_cell_volume                     2748.9(3)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      133(4)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -10.00   86.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372   77.0000  -60.0000 96

  2 omega   14.00   60.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -99.0000 -180.0000 46

  3 omega  -86.00  -28.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8185  145.0000  -27.0470 58

  4 omega  -61.00   49.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8185   19.0000  120.0000 110

  5 omega  -40.00   50.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8185   57.0000 -180.0000 90
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0321007000
_diffrn_orient_matrix_UB_12      0.0416001000
_diffrn_orient_matrix_UB_13      0.0093676000
_diffrn_orient_matrix_UB_21      -0.0829762000
_diffrn_orient_matrix_UB_22      0.0071353000
_diffrn_orient_matrix_UB_23      0.0142546000
_diffrn_orient_matrix_UB_31      0.0345637000
_diffrn_orient_matrix_UB_32      -0.0234203000
_diffrn_orient_matrix_UB_33      0.0224720000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_unetI/netI     0.1264
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19253
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.83
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63049
_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
;
;
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1280
_refine_diff_density_max         2.173
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         9657
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1405
_refine_ls_R_factor_gt           0.1095
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+47.9301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2399
_refine_ls_wR_factor_ref         0.2571
_reflns_number_gt                7091
_reflns_number_total             9657
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg500942g_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4512213--4512215.cif.'
_cod_database_code               4512213
_chemical_oxdiff_formula         'C Zn'
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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,H) groups
2. Rigid bond restraints
 C77, C52, C44, C89, C154, C132
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Rotating group:
 O13(H13a,H13b), O45(H45a,H45b)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C44(H44), C50(H50), C52(H52), C54(H54), C56(H56), C58(H58), C65(H65),
 C67(H67), C72(H72), C80(H80), C88(H88), C92(H92), C102(H102), C104(H104),
 C106(H106), C110(H110), C116(H116), C118(H118), C122(H122), C124(H124),
 C125(H125), C128(H128), C129(H129), C132(H132), C143(H143), C151(H151),
 C154(H154)
3.c Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C36(H36a,H36b,H36c), C41(H41a,H41b,H41c), C73(H73a,H73b,
 H73c), C76(H76a,H76b,H76c), C84(H84a,H84b,H84c), C86(H86a,H86b,H86c),
 C158(H15a,H15b,H15c), C2(H2a,H2b,H2c)
;
_olex2_submission_special_instructions 'No special instructions were received'