#------------------------------------------------------------------------------
#$Date: 2019-11-24 06:06:24 +0200 (Sun, 24 Nov 2019) $
#$Revision: 236902 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/98/4349867.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4349867
loop_
_publ_author_name
'Wang, Yutong'
'Fan, Weidong'
'Wang, Xia'
'Han, Yinfeng'
'Zhang, Liangliang'
'Liu, Di'
'Dai, Fangna'
'Sun, Daofeng'
_publ_section_title
;
 Solvent-induced framework-interpenetration isomers of Cu MOFs for
 efficient light hydrocarbon separation
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              2408
_journal_paper_doi               10.1039/C8QI00469B
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         '0.13(C400 H208 Cu24 O120)'
_chemical_formula_sum            'C50 H26 Cu3 O15'
_chemical_formula_weight         1057.33
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_Hall           '-I 4 2c'
_space_group_name_H-M_alt        'I 4/m c m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-02 deposited with the CCDC.
2018-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.3382(11)
_cell_length_b                   31.3382(11)
_cell_length_c                   39.0786(10)
_cell_measurement_reflns_used    3093
_cell_measurement_temperature    273.45(10)
_cell_measurement_theta_max      46.5040
_cell_measurement_theta_min      4.4500
_cell_volume                     38378(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      273.45(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00   4.00   1.00    4.04    --    0.00  97.00-130.00   29
  2  ω    -21.00  16.00   1.00    4.04    --    0.00  61.00 133.00   37
  3  ω     23.00 112.00   1.00   16.16    --   54.00-125.00  30.00   89
  4  ω     91.00 121.00   1.00   16.16    --   54.00  77.00 150.00   30
  5  ω     25.00  74.00   1.00   16.16    --   54.00-125.00-180.00   49
  6  ω    139.00 166.00   1.00   16.16    --  108.00  97.00-130.00   27
  7  ω    100.00 178.00   1.00   16.16    --  108.00 111.00 -60.00   78
  8  ω    114.00 163.00   1.00   16.16    --  108.00 111.00 -90.00   49
  9  ω     81.00 178.00   1.00   16.16    --  108.00  77.00 -30.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0460262000
_diffrn_orient_matrix_UB_12      0.0152757000
_diffrn_orient_matrix_UB_13      0.0066609000
_diffrn_orient_matrix_UB_21      0.0038614000
_diffrn_orient_matrix_UB_22      0.0317918000
_diffrn_orient_matrix_UB_23      -0.0298758000
_diffrn_orient_matrix_UB_31      -0.0170025000
_diffrn_orient_matrix_UB_32      -0.0341271000
_diffrn_orient_matrix_UB_33      -0.0248794000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_unetI/netI     0.1119
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            34407
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.059
_diffrn_reflns_theta_max         67.059
_diffrn_reflns_theta_min         3.616
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.366
_exptl_crystal_description       block
_exptl_crystal_F_000             4264
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.030
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.731
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         8965
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.731
_refine_ls_R_factor_all          0.1478
_refine_ls_R_factor_gt           0.0640
_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/[σ²(Fo²)+(0.0524P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2543
_reflns_number_total             8965
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8qi00469b2.cif
_cod_data_source_block           UPC-35
_cod_original_cell_volume        38378(3)
_cod_database_code               4349867
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N Cu'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.949
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H1A(0.25) H1B(0.25) H2A(0.25) H2B(0.25)
3.a Rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C4(H4), C3(H3), C5(H5), C11(H11), C7(H7)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.251
_oxdiff_exptl_absorpt_empirical_full_min 0.674
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'x, -y, -z+1/2'
'-x, -y, z'
'-y, -x, -z+1/2'
'y, x, -z+1/2'
'y, -x, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, -x+1/2, -z+1'
'y+1/2, x+1/2, -z+1'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'y, -x, -z'
'-x, y, z-1/2'
'x, y, -z'
'y, x, z-1/2'
'-y, -x, z-1/2'
'-y, x, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, x+1/2, z'
'-y+1/2, -x+1/2, z'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.37931(2) 0.12069(2) 0.0000 0.1084(4) Uani 1 4 d S T P
Cu3 Cu 0.0000 0.0000 0.21597(2) 0.1056(4) Uani 1 4 d S T P
Cu2 Cu 0.31960(3) 0.18040(3) 0.0000 0.1141(4) Uani 1 4 d S T P
O6 O 0.0000 0.0000 0.16086(9) 0.1133(14) Uani 1 4 d S T P
O5 O 0.06188(7) 0.00686(7) 0.22200(5) 0.1129(8) Uani 1 1 d . . .
O4 O 0.34392(9) 0.09381(8) 0.03570(5) 0.1175(9) Uani 1 1 d . . .
O3 O 0.29285(8) 0.14574(9) 0.03535(5) 0.1227(9) Uani 1 1 d . . .
O1 O 0.42772(11) 0.07228(11) 0.0000 0.1359(17) Uani 1 4 d S T P
H1A H 0.4544 0.0584 0.0234 0.204 Uiso 0.25 1 d GR . .
H1B H 0.4404 0.0443 -0.0230 0.204 Uiso 0.25 1 d GR . .
O2 O 0.27133(12) 0.22867(12) 0.0000 0.1517(19) Uani 1 4 d S T P
H2A H 0.2454 0.2321 0.0156 0.228 Uiso 0.25 1 d GR . .
H2B H 0.2685 0.2550 -0.0152 0.228 Uiso 0.25 1 d GR . .
C13 C 0.12764(19) 0.0000 0.2500 0.1179(18) Uani 1 2 d S T P
C1 C 0.31151(14) 0.11300(15) 0.04599(9) 0.1045(12) Uani 1 1 d . . .
C2 C 0.28935(13) 0.09010(14) 0.07695(9) 0.1098(12) Uani 1 1 d . . .
C12 C 0.15009(14) 0.01261(13) 0.22064(9) 0.1400(16) Uani 1 1 d . . .
H12 H 0.1354 0.0218 0.2013 0.168 Uiso 1 1 calc R . .
C14 C 0.0812(2) 0.0000 0.2500 0.132(2) Uani 1 2 d S T P
C4 C 0.30925(14) 0.05541(16) 0.09160(10) 0.1551(18) Uani 1 1 d . . .
H4 H 0.3345 0.0442 0.0829 0.186 Uiso 1 1 calc R . .
C3 C 0.25273(15) 0.10846(15) 0.08909(9) 0.1500(17) Uani 1 1 d . . .
H3 H 0.2406 0.1320 0.0783 0.180 Uiso 1 1 calc R . .
C5 C 0.28864(16) 0.03770(18) 0.12113(11) 0.174(2) Uani 1 1 d . . .
H5 H 0.3000 0.0135 0.1314 0.209 Uiso 1 1 calc R . .
C10 C 0.19325(16) 0.01131(16) 0.22068(9) 0.1567(18) Uani 1 1 d . . .
C8 C 0.23235(14) 0.03820(16) 0.16526(10) 0.1592(19) Uani 1 1 d . . .
C9 C 0.21617(13) 0.02580(17) 0.19025(10) 0.1663(19) Uani 1 1 d . . .
C11 C 0.21760(18) 0.0000 0.2500 0.173(3) Uani 1 2 d S T P
H11 H 0.2473 0.0000 0.2500 0.208 Uiso 1 2 calc RS T P
C7 C 0.23377(14) 0.09021(18) 0.11902(11) 0.178(2) Uani 1 1 d . . .
H7 H 0.2088 0.1018 0.1278 0.214 Uiso 1 1 calc R . .
C6 C 0.25196(17) 0.05617(18) 0.13458(10) 0.1446(17) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O4 Cu1 Cu2 84.51(9) 30 .
O4 Cu1 Cu2 84.50(9) . .
O4 Cu1 Cu2 84.51(9) 20 .
O4 Cu1 Cu2 84.51(9) 13_554 .
O4 Cu1 O4 90.10(13) 30 13_554
O4 Cu1 O4 88.85(13) 30 .
O4 Cu1 O4 90.10(13) . 20
O4 Cu1 O4 169.01(18) 30 20
O4 Cu1 O4 88.85(13) 13_554 20
O4 Cu1 O4 169.01(18) 13_554 .
O4 Cu1 O1 95.49(9) 30 .
O4 Cu1 O1 95.49(9) 20 .
O4 Cu1 O1 95.49(9) 13_554 .
O4 Cu1 O1 95.50(9) . .
O1 Cu1 Cu2 180.00(14) . .
O6 Cu3 Cu3 180.0 . 3
O5 Cu3 Cu3 83.11(6) 7 3
O5 Cu3 Cu3 83.11(6) 4 3
O5 Cu3 Cu3 83.11(6) 2 3
O5 Cu3 Cu3 83.11(6) . 3
O5 Cu3 O6 96.89(6) . .
O5 Cu3 O6 96.89(6) 7 .
O5 Cu3 O6 96.89(6) 2 .
O5 Cu3 O6 96.89(6) 4 .
O5 Cu3 O5 89.175(14) 2 .
O5 Cu3 O5 89.177(14) 7 .
O5 Cu3 O5 166.22(12) 4 .
O5 Cu3 O5 89.176(14) 4 2
O5 Cu3 O5 166.22(12) 2 7
O5 Cu3 O5 89.176(14) 4 7
O3 Cu2 Cu1 84.84(9) 20 .
O3 Cu2 Cu1 84.84(9) 13_554 .
O3 Cu2 Cu1 84.84(9) . .
O3 Cu2 Cu1 84.84(9) 30 .
O3 Cu2 O3 169.69(18) . 13_554
O3 Cu2 O3 88.69(15) 20 13_554
O3 Cu2 O3 90.39(15) . 20
O3 Cu2 O3 169.69(18) 30 20
O3 Cu2 O3 90.39(15) 30 13_554
O3 Cu2 O3 88.68(15) . 30
O3 Cu2 O2 95.16(9) 20 .
O3 Cu2 O2 95.16(9) 13_554 .
O3 Cu2 O2 95.16(9) 30 .
O3 Cu2 O2 95.16(9) . .
O2 Cu2 Cu1 180.00(15) . .
C14 O5 Cu3 123.8(3) . .
C1 O4 Cu1 118.7(3) . .
C1 O3 Cu2 119.4(3) . .
C12 C13 C12 119.8(5) . 3
C12 C13 C14 120.1(3) 3 .
C12 C13 C14 120.1(3) . .
O4 C1 O3 132.0(4) . .
O4 C1 C2 112.9(4) . .
O3 C1 C2 115.1(4) . .
C4 C2 C1 118.7(4) . .
C3 C2 C1 116.5(4) . .
C3 C2 C4 124.5(4) . .
C10 C12 C13 119.5(4) . .
O5 C14 O5 123.0(6) . 3
O5 C14 C13 118.5(3) . .
O5 C14 C13 118.5(3) 3 .
C2 C4 C5 115.8(4) . .
C2 C3 C7 117.6(4) . .
C6 C5 C4 121.0(5) . .
C12 C10 C9 118.8(4) . .
C12 C10 C11 123.0(4) . .
C11 C10 C9 118.0(4) . .
C9 C8 C6 176.8(6) . .
C8 C9 C10 176.2(5) . .
C10 C11 C10 115.1(5) . 3
C6 C7 C3 120.5(4) . .
C5 C6 C8 119.9(5) . .
C7 C6 C5 120.4(4) . .
C7 C6 C8 119.7(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 Cu2 2.6462(16) .
Cu1 O4 1.972(2) 20
Cu1 O4 1.971(2) .
Cu1 O4 1.972(2) 13_554
Cu1 O4 1.972(2) 30
Cu1 O1 2.145(5) .
Cu3 Cu3 2.6599(15) 3
Cu3 O6 2.154(4) .
Cu3 O5 1.965(2) 7
Cu3 O5 1.965(2) .
Cu3 O5 1.965(2) 4
Cu3 O5 1.965(2) 2
Cu2 O3 1.947(2) .
Cu2 O3 1.947(2) 20
Cu2 O3 1.947(2) 13_554
Cu2 O3 1.947(2) 30
Cu2 O2 2.140(5) .
O5 C14 1.269(3) .
O4 C1 1.247(4) .
O3 C1 1.252(4) .
C13 C12 1.403(4) .
C13 C12 1.403(4) 3
C13 C14 1.455(6) .
C1 C2 1.569(5) .
C2 C4 1.378(5) .
C2 C3 1.369(4) .
C12 C10 1.353(5) .
C14 O5 1.269(3) 3
C4 C5 1.434(5) .
C3 C7 1.431(5) .
C5 C6 1.390(5) .
C10 C9 1.461(5) .
C10 C11 1.422(5) .
C8 C9 1.167(5) .
C8 C6 1.461(5) .
C11 C10 1.422(5) 3
C7 C6 1.354(5) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.001 -0.006 -0.004 31798 6412 ' '
