#------------------------------------------------------------------------------
#$Date: 2019-11-24 02:38:50 +0200 (Sun, 24 Nov 2019) $
#$Revision: 236298 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/65/7236547.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_7236547
loop_
_publ_author_name
'Grancha, Thais'
'Mon, Marta'
'Ferrando-Soria, Jesús'
'Gascon, Jorge'
'Seoane, Beatriz'
'Ramos-Fernandez, Enrique V.'
'Armentano, Donatella'
'Pardo, Emilio'
_publ_section_title
;
 Tuning the selectivity of light hydrocarbons in natural gas in a family
 of isoreticular MOFs
;
_journal_issue                   22
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              11032
_journal_paper_doi               10.1039/C7TA01179B
_journal_volume                  5
_journal_year                    2017
_chemical_formula_sum            'C36 H78 Ca Cu6 N6 O34'
_chemical_formula_weight         1560.36
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-02-01 deposited with the CCDC.
2017-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   17.783(3)
_cell_length_b                   17.783(3)
_cell_length_c                   12.889(2)
_cell_measurement_reflns_used    1896
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      2.25
_cell_volume                     3529.9(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    CrystalMaker
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2169
_diffrn_reflns_av_unetI/netI     0.2253
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20336
_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         24.998
_diffrn_reflns_theta_min         1.322
_exptl_absorpt_coefficient_mu    1.930
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       hexagonal/prism
_exptl_crystal_F_000             1604
_exptl_crystal_preparation       ', porous'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: slow diffusion of 1:1 H2O:CH3OH solutions '
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.101
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.309
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.37(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         4076
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.2383
_refine_ls_R_factor_gt           0.0960
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1600P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2290
_refine_ls_wR_factor_ref         0.3194
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                1687
_reflns_number_total             4076
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ta01179b2.cif
_cod_data_source_block           1
_cod_original_cell_volume        3529.7(11)
_cod_database_code               7236547
_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.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
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 0.8632(3) 0.4171(3) 0.2343(2) 0.0369(19) Uani 1 1 d . . .
Cu2 Cu 0.8627(3) 0.4197(3) 0.4952(2) 0.039(2) Uani 1 1 d . . .
Ca1 Ca 0.6667 0.3333 0.3642(18) 0.0192(15) Uani 1 3 d S T P
O1H O 0.8235(8) 0.3578(8) 0.363(3) 0.031(3) Uani 1 1 d . . .
O1 O 0.9741(18) 0.4182(18) 0.219(3) 0.046(9) Uani 1 1 d . . .
O2 O 0.7611(16) 0.4394(15) 0.232(2) 0.038(8) Uani 1 1 d . . .
O3 O 0.804(2) 0.288(3) 0.149(3) 0.17(2) Uani 1 1 d . . .
O4 O 0.7659(18) 0.441(2) 0.497(2) 0.043(8) Uani 1 1 d . . .
O5 O 0.7977(19) 0.2928(18) 0.5895(18) 0.049(7) Uiso 1 1 d . . .
O6 O 0.9823(17) 0.429(2) 0.514(2) 0.040(8) Uani 1 1 d . . .
N1 N 0.9059(19) 0.509(2) 0.127(2) 0.032(8) Uiso 1 1 d D . .
N2 N 0.902(2) 0.497(3) 0.605(4) 0.087(17) Uani 1 1 d D . .
C1 C 0.978(3) 0.527(3) 0.088(4) 0.042(13) Uani 1 1 d . . .
C2 C 1.017(3) 0.479(3) 0.142(4) 0.037(12) Uiso 1 1 d . . .
C3 C 0.7676(19) 0.4925(19) 0.160(2) 0.019(7) Uiso 1 1 d . . .
C4 C 0.763(3) 0.485(5) 0.575(6) 0.19(4) Uani 1 1 d . . .
C5 C 0.859(3) 0.551(2) 0.622(3) 0.065(12) Uiso 1 1 d D . .
H5 H 0.8483 0.5459 0.6983 0.078 Uiso 1 1 calc R U .
C6 C 0.895(2) 0.647(2) 0.601(3) 0.080(12) Uiso 1 1 d D . .
H6 H 0.9544 0.6773 0.6332 0.096 Uiso 1 1 calc R U .
C7 C 0.909(3) 0.668(3) 0.488(3) 0.108(15) Uiso 1 1 d D . .
H7A H 0.9397 0.6403 0.4581 0.162 Uiso 1 1 calc R U .
H7B H 0.9431 0.7306 0.4789 0.162 Uiso 1 1 calc R U .
H7C H 0.8524 0.6453 0.4542 0.162 Uiso 1 1 calc R U .
C8 C 0.844(4) 0.687(4) 0.655(5) 0.16(2) Uiso 1 1 d D . .
H8A H 0.8725 0.7493 0.6388 0.243 Uiso 1 1 calc R U .
H8B H 0.8441 0.6793 0.7301 0.243 Uiso 1 1 calc R U .
H8C H 0.7844 0.6580 0.6292 0.243 Uiso 1 1 calc R U .
C9 C 0.843(2) 0.533(3) 0.086(2) 0.067(13) Uiso 1 1 d D . .
H9 H 0.8700 0.5972 0.0891 0.080 Uiso 1 1 calc R U .
C10 C 0.8030 0.5016 -0.0245 0.278 Uiso 1 1 d D . .
H10 H 0.7432 0.4564 -0.0027 0.333 Uiso 1 1 calc R U .
C11 C 0.826(6) 0.442(5) -0.089(6) 0.31(6) Uiso 1 1 d D . .
H11A H 0.8301 0.4005 -0.0424 0.466 Uiso 1 1 calc R U .
H11B H 0.8825 0.4779 -0.1231 0.466 Uiso 1 1 calc R U .
H11C H 0.7815 0.4109 -0.1411 0.466 Uiso 1 1 calc R U .
C12 C 0.780(5) 0.572(5) -0.071(7) 0.32(6) Uiso 1 1 d D . .
H12A H 0.7322 0.5435 -0.1211 0.482 Uiso 1 1 calc R U .
H12B H 0.8309 0.6186 -0.1053 0.482 Uiso 1 1 calc R U .
H12C H 0.7617 0.5963 -0.0142 0.482 Uiso 1 1 calc R U .
O1W O 0.3045(15) 0.3327(15) 0.865(4) 0.108(7) Uiso 1 1 d . . .
O2W O 0.983(4) 0.155(4) 0.362(8) 0.29(2) Uiso 1 1 d . . .
O3W O 0.969(8) 0.843(8) 0.129(11) 0.51(7) Uiso 1 1 d . . .
O4W O 0.878(6) 0.885(6) -0.060(6) 0.36(4) Uiso 1 1 d . . .
O5W O 1.0000 1.0000 0.23(2) 0.8(2) Uiso 1 3 d S . P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 '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
O1H Cu1 O1 100.5(11) . .
O1H Cu1 N1 162.0(11) . .
O1 Cu1 N1 87.3(13) . .
O1H Cu1 O2 90.1(9) . .
O1 Cu1 O2 168.0(13) . .
N1 Cu1 O2 81.0(12) . .
O1H Cu1 O3 90.5(13) . .
O1 Cu1 O3 85.3(13) . .
N1 Cu1 O3 106.4(15) . .
O2 Cu1 O3 100.5(13) . .
O1H Cu1 Ca1 47.7(5) . .
O1 Cu1 Ca1 147.1(10) . .
N1 Cu1 Ca1 125.6(9) . .
O2 Cu1 Ca1 44.6(8) . .
O3 Cu1 Ca1 86.8(7) . .
N2 Cu2 O4 83.4(13) . .
N2 Cu2 O1H 168.7(16) . .
O4 Cu2 O1H 91.3(10) . .
N2 Cu2 O6 81.8(13) . .
O4 Cu2 O6 164.2(14) . .
O1H Cu2 O6 102.2(9) . .
N2 Cu2 O5 98.1(17) . .
O4 Cu2 O5 97.2(11) . .
O1H Cu2 O5 92.6(8) . .
O6 Cu2 O5 90.4(12) . .
N2 Cu2 Ca1 128.7(10) . .
O4 Cu2 Ca1 45.6(9) . .
O1H Cu2 Ca1 48.0(5) . .
O6 Cu2 Ca1 149.5(9) . .
O5 Cu2 Ca1 85.5(7) . .
O2 Ca1 O2 77.7(12) . 3_665
O2 Ca1 O2 77.7(12) . 2_655
O2 Ca1 O2 77.7(12) 3_665 2_655
O2 Ca1 O4 138.4(10) . 3_665
O2 Ca1 O4 86.5(5) 3_665 3_665
O2 Ca1 O4 136.2(10) 2_655 3_665
O2 Ca1 O4 86.5(5) . .
O2 Ca1 O4 136.2(10) 3_665 .
O2 Ca1 O4 138.4(10) 2_655 .
O4 Ca1 O4 78.7(12) 3_665 .
O2 Ca1 O4 136.2(10) . 2_655
O2 Ca1 O4 138.4(10) 3_665 2_655
O2 Ca1 O4 86.5(5) 2_655 2_655
O4 Ca1 O4 78.7(12) 3_665 2_655
O4 Ca1 O4 78.7(12) . 2_655
O2 Ca1 O1H 66.8(9) . .
O2 Ca1 O1H 70.3(8) 3_665 .
O2 Ca1 O1H 136.1(12) 2_655 .
O4 Ca1 O1H 71.6(8) 3_665 .
O4 Ca1 O1H 65.9(9) . .
O4 Ca1 O1H 137.2(13) 2_655 .
O2 Ca1 O1H 136.1(12) . 3_665
O2 Ca1 O1H 66.8(9) 3_665 3_665
O2 Ca1 O1H 70.3(8) 2_655 3_665
O4 Ca1 O1H 65.9(9) 3_665 3_665
O4 Ca1 O1H 137.2(13) . 3_665
O4 Ca1 O1H 71.6(8) 2_655 3_665
O1H Ca1 O1H 119.998(17) . 3_665
O2 Ca1 O1H 70.3(8) . 2_655
O2 Ca1 O1H 136.1(12) 3_665 2_655
O2 Ca1 O1H 66.8(9) 2_655 2_655
O4 Ca1 O1H 137.2(13) 3_665 2_655
O4 Ca1 O1H 71.6(8) . 2_655
O4 Ca1 O1H 65.9(9) 2_655 2_655
O1H Ca1 O1H 120.00(2) . 2_655
O1H Ca1 O1H 120.00(2) 3_665 2_655
O2 Ca1 Cu2 103.3(6) . 2_655
O2 Ca1 Cu2 158.3(8) 3_665 2_655
O2 Ca1 Cu2 81.3(7) 2_655 2_655
O4 Ca1 Cu2 105.1(9) 3_665 2_655
O4 Ca1 Cu2 65.1(6) . 2_655
O4 Ca1 Cu2 33.4(6) 2_655 2_655
O1H Ca1 Cu2 130.5(7) . 2_655
O1H Ca1 Cu2 100.8(5) 3_665 2_655
O1H Ca1 Cu2 34.0(7) 2_655 2_655
O2 Ca1 Cu2 81.3(7) . .
O2 Ca1 Cu2 103.3(6) 3_665 .
O2 Ca1 Cu2 158.3(8) 2_655 .
O4 Ca1 Cu2 65.1(6) 3_665 .
O4 Ca1 Cu2 33.4(6) . .
O4 Ca1 Cu2 105.1(9) 2_655 .
O1H Ca1 Cu2 34.0(7) . .
O1H Ca1 Cu2 130.5(7) 3_665 .
O1H Ca1 Cu2 100.8(5) 2_655 .
Cu2 Ca1 Cu2 98.3(5) 2_655 .
O2 Ca1 Cu2 158.3(8) . 3_665
O2 Ca1 Cu2 81.3(7) 3_665 3_665
O2 Ca1 Cu2 103.3(6) 2_655 3_665
O4 Ca1 Cu2 33.4(6) 3_665 3_665
O4 Ca1 Cu2 105.2(9) . 3_665
O4 Ca1 Cu2 65.1(6) 2_655 3_665
O1H Ca1 Cu2 100.8(5) . 3_665
O1H Ca1 Cu2 34.0(7) 3_665 3_665
O1H Ca1 Cu2 130.5(7) 2_655 3_665
Cu2 Ca1 Cu2 98.3(5) 2_655 3_665
Cu2 Ca1 Cu2 98.3(5) . 3_665
Cu1 O1H Cu2 121.2(6) . .
Cu1 O1H Ca1 99.6(10) . .
Cu2 O1H Ca1 98.0(10) . .
C2 O1 Cu1 104(3) . .
C3 O2 Cu1 113(2) . .
C3 O2 Ca1 147(2) . .
Cu1 O2 Ca1 99.9(11) . .
C3 O3 Cu1 121(2) 3_665 .
C4 O4 Cu2 116(3) . .
C4 O4 Ca1 140(3) . .
Cu2 O4 Ca1 101.0(12) . .
C4 O5 Cu2 122(3) 3_665 .
C1 O6 Cu2 113(3) 4_765 .
C1 N1 C9 127(4) . .
C1 N1 Cu1 115(3) . .
C9 N1 Cu1 117(3) . .
C2 N2 C5 123(4) 4_765 .
C2 N2 Cu2 116(3) 4_765 .
C5 N2 Cu2 117(3) . .
O6 C1 N1 132(5) 4_764 .
O6 C1 C2 117(3) 4_764 .
N1 C1 C2 111(3) . .
N2 C2 O1 125(4) 4_764 .
N2 C2 C1 112(3) 4_764 .
O1 C2 C1 123(3) . .
O3 C3 O2 122(3) 2_655 .
O3 C3 C9 116(3) 2_655 .
O2 C3 C9 123(3) . .
O5 C4 O4 125(5) 2_655 .
O5 C4 C5 116(4) 2_655 .
O4 C4 C5 112(4) . .
N2 C5 C6 129(4) . .
N2 C5 C4 100(3) . .
C6 C5 C4 117(4) . .
C7 C6 C5 112(3) . .
C7 C6 C8 112(4) . .
C5 C6 C8 115(4) . .
N1 C9 C3 105(3) . .
N1 C9 C10 120(3) . .
C3 C9 C10 106(2) . .
C11 C10 C9 120(4) . .
C11 C10 C12 126(5) . .
C9 C10 C12 108(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1H 1.90(3) .
Cu1 O1 1.97(3) .
Cu1 N1 1.98(3) .
Cu1 O2 2.04(3) .
Cu1 O3 2.27(3) .
Cu1 Ca1 3.468(12) .
Cu2 N2 1.85(4) .
Cu2 O4 1.94(2) .
Cu2 O1H 1.96(3) .
Cu2 O6 2.07(3) .
Cu2 O5 2.30(3) .
Cu2 Ca1 3.465(13) .
Ca1 O2 2.47(3) .
Ca1 O2 2.47(3) 3_665
Ca1 O2 2.47(3) 2_655
Ca1 O4 2.52(3) 3_665
Ca1 O4 2.52(3) .
Ca1 O4 2.52(3) 2_655
Ca1 O1H 2.600(12) .
Ca1 O1H 2.600(12) 3_665
Ca1 O1H 2.600(12) 2_655
Ca1 Cu2 3.465(13) 2_655
Ca1 Cu2 3.465(13) 3_665
O1 C2 1.38(5) .
O2 C3 1.29(4) .
O3 C3 1.27(4) 3_665
O4 C4 1.28(6) .
O5 C4 1.22(6) 3_665
O6 C1 1.20(5) 4_765
N1 C1 1.26(5) .
N1 C9 1.48(2) .
N2 C2 1.37(5) 4_765
N2 C5 1.509(19) .
C1 O6 1.20(5) 4_764
C1 C2 1.51(3) .
C2 N2 1.37(5) 4_764
C3 O3 1.27(4) 2_655
C3 C9 1.51(5) .
C4 O5 1.22(6) 2_655
C4 C5 1.62(6) .
C5 C6 1.53(2) .
C6 C7 1.49(2) .
C6 C8 1.56(3) .
C9 C10 1.56(3) .
C10 C11 1.55(4) .
C10 C12 1.62(4) .
