A three-dimensional metal‒organic framework for a guest-free ultra-low dielectric material
Xu, W.; Yu, S. S.; Zhang, H.; Duan, H. B.; RSC Advances 9 (2019) 16183–; doi:10.1039/C9RA03032H

data_7232822
_publ_section_title
;
 A three-dimensional metal--organic framework for a guest-free ultra-low
 dielectric material
;
_journal_issue                   28
_journal_name_full               'RSC Advances'
_journal_page_first              16183
_journal_paper_doi               10.1039/C9RA03032H
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C112 H64 O32 Zn6, 4(C2 H8 N)'
_chemical_formula_sum            'C120 H96 N4 O32 Zn6'
_chemical_formula_weight         2498.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-11-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-12 deposited with the CCDC.    2019-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.7046(12)
_cell_length_b                   14.5230(9)
_cell_length_c                   22.3879(12)
_cell_measurement_reflns_used    5954
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      25.7620
_cell_measurement_theta_min      2.3050
_cell_volume                     8032.4(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     40.00  80.00   1.00    6.50    --   11.74-178.00  60.00   40
  2  \w     34.00  64.00   1.00    6.50    --   11.74-178.00 150.00   30
  3  \w    -45.00  44.00   1.00    6.50    --   11.74 -77.00-150.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0119460000
_diffrn_orient_matrix_UB_12      0.0234341000
_diffrn_orient_matrix_UB_13      -0.0180140000
_diffrn_orient_matrix_UB_21      0.0397568000
_diffrn_orient_matrix_UB_22      -0.0062310000
_diffrn_orient_matrix_UB_23      -0.0156815000
_diffrn_orient_matrix_UB_31      -0.0256936000
_diffrn_orient_matrix_UB_32      -0.0204138000
_diffrn_orient_matrix_UB_33      -0.0159309000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27445
_diffrn_reflns_point_group_measured_fraction_full 0.853
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.164
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
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    1.033
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.852
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         12067
_refine_ls_number_restraints     615
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0884
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1273P)^2^+48.4203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2323
_refine_ls_wR_factor_ref         0.2429
_reflns_Friedel_coverage         0.662
_reflns_Friedel_fraction_full    0.699
_reflns_Friedel_fraction_max     0.699
_reflns_number_gt                10124
_reflns_number_total             12067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra03032h2.cif
_cod_data_source_block           nj03_sq
_cod_database_code               7232822
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.920
_shelx_estimated_absorpt_t_min   0.896
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53(3)
 0.47(3)
2. 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
3. Restrained distances
 C28-C25
 1.4 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O11) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6.a Secondary CH2 refined with riding coordinates:
 N2S(H2SA,H2SB), N3S(H3SD,H3SE)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27),
  C31(H31), C32(H32), C34(H34), C35(H35), C37(H37), C38(H38), C40(H40),
 C41(H41), C45(H45), C46(H46), C48(H48), C49(H49), C51(H51), C52(H52), C54(H54),
  C55(H55)
6.c Idealised Me refined as rotating group:
 C3S(H3SA,H3SB,H3SC), C4S(H4SA,H4SB,H4SC), C5S(H5SA,H5SB,H5SC), C6S(H6SA,H6SB,
 H6SC)
;
_shelx_res_checksum              68936
_shelx_fab_checksum              14212
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.519
_oxdiff_exptl_absorpt_empirical_full_min 0.811