#------------------------------------------------------------------------------
#$Date: 2019-11-22 19:07:30 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231278 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/63/4516379.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_4516379
loop_
_publ_author_name
'Luo, Xiaolong'
'Sun, Libo'
'Zhao, Jun'
'Li, Dong-Sheng'
'Wang, Dongmei'
'Li, Guanghua'
'Huo, Qisheng'
'Liu, Yunling'
_publ_section_title
;
 Three Metal--Organic Frameworks Based on Binodal Inorganic Building Units
 and Hetero-O, N Donor Ligand: Solvothermal Syntheses, Structures, and Gas
 Sorption Properties
;
_journal_issue                   10
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4901
_journal_paper_doi               10.1021/acs.cgd.5b00791
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C63 H84 Cu7 I4 N11 O23'
_chemical_formula_sum            'C63 H84 Cu7 I4 N11 O23'
_chemical_formula_weight         2315.79
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   27.538(4)
_cell_length_b                   27.538(4)
_cell_length_c                   20.139(4)
_cell_measurement_temperature    293(2)
_cell_volume                     13226(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1080
_diffrn_reflns_av_unetI/netI     0.0915
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            93448
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.033
_exptl_absorpt_coefficient_mu    2.084
_exptl_absorpt_correction_T_max  0.5241
_exptl_absorpt_correction_T_min  0.4715
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       block
_exptl_crystal_F_000             4552
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.137
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         10349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_gt           0.0509
_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/[σ²(Fo²)+(0.0700P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5109
_reflns_number_total             10349
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00791_si_003.cif
_cod_data_source_block           JLU_Liu16
_cod_original_cell_volume        13225(5)
_cod_database_code               4516379
_shelx_shelxl_version_number     2014/7
_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.
;
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'
'-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
I1 I 0.22672(2) 0.63420(2) 0.54931(2) 0.07935(17) Uani 1 1 d . . .
I2 I 0.3333 0.6667 0.36496(3) 0.0733(2) Uani 1 3 d S T P
Cu1 Cu 0.28777(3) 0.60524(3) 0.47476(4) 0.0777(2) Uani 1 1 d . . .
Cu2 Cu 0.3333 0.6667 0.58258(6) 0.0816(4) Uani 1 3 d S T P
Cu3 Cu 0.23443(3) 0.33287(3) 0.2500 0.0449(2) Uani 1 2 d S T P
Cu4 Cu 0.32881(3) 0.43117(3) 0.2500 0.0420(2) Uani 1 2 d S T P
O1 O 0.21137(14) 0.36887(14) 0.31983(16) 0.0559(9) Uani 1 1 d . . .
O2 O 0.29103(15) 0.45132(14) 0.31759(17) 0.0695(11) Uani 1 1 d . . .
O3 O -0.04092(14) 0.27229(15) 0.68097(17) 0.0626(9) Uani 1 1 d . . .
O4 O -0.04542(15) 0.35125(15) 0.68229(19) 0.0753(11) Uani 1 1 d . . .
O5 O 0.1582(2) 0.2548(2) 0.2500 0.110(2) Uani 1 2 d S T P
O6 O 0.4049(2) 0.5157(3) 0.2500 0.101(2) Uani 1 2 d S T P
N1 N 0.23769(19) 0.52387(18) 0.4501(2) 0.0682(13) Uani 1 1 d . . .
N2 N 0.3333 0.6667 0.6854(4) 0.077(2) Uani 1 3 d S T P
C1 C 0.2515(2) 0.4981(2) 0.4032(2) 0.0609(14) Uani 1 1 d . . .
H1 H 0.2836 0.5199 0.3781 0.073 Uiso 1 1 calc R U .
C2 C 0.2208(2) 0.4410(2) 0.3900(2) 0.0511(12) Uani 1 1 d . . .
C3 C 0.1737(2) 0.4080(2) 0.4275(2) 0.0572(13) Uani 1 1 d . . .
H3 H 0.1525 0.3696 0.4200 0.069 Uiso 1 1 calc R U .
C4 C 0.1585(2) 0.4333(2) 0.4770(3) 0.0675(15) Uani 1 1 d . . .
C5 C 0.1917(2) 0.4905(3) 0.4857(3) 0.0802(19) Uani 1 1 d . . .
H5 H 0.1815 0.5072 0.5188 0.096 Uiso 1 1 calc R U .
C6 C 0.2423(2) 0.4178(2) 0.3384(2) 0.0489(12) Uani 1 1 d . . .
C7 C 0.1079(2) 0.4023(2) 0.5203(3) 0.0732(17) Uani 1 1 d . . .
C8 C 0.0929(2) 0.3493(3) 0.5420(3) 0.0835(19) Uani 1 1 d . . .
H8 H 0.1120 0.3315 0.5271 0.100 Uiso 1 1 calc R U .
C9 C 0.0479(2) 0.3223(2) 0.5871(3) 0.0792(18) Uani 1 1 d . . .
H9 H 0.0371 0.2861 0.6014 0.095 Uiso 1 1 calc R U .
C10 C 0.0196(2) 0.3488(2) 0.6108(3) 0.0647(15) Uani 1 1 d . . .
C11 C 0.0336(3) 0.4008(3) 0.5858(3) 0.088(2) Uani 1 1 d . . .
H11 H 0.0136 0.4182 0.5989 0.106 Uiso 1 1 calc R U .
C12 C 0.0776(3) 0.4271(3) 0.5410(3) 0.091(2) Uani 1 1 d . . .
H12 H 0.0868 0.4622 0.5245 0.109 Uiso 1 1 calc R U .
C13 C -0.0264(2) 0.3214(3) 0.6624(3) 0.0605(14) Uani 1 1 d . . .
C14 C 0.3901(2) 0.6864(3) 0.7115(3) 0.0851(18) Uani 1 1 d . . .
H14A H 0.4152 0.7241 0.6955 0.102 Uiso 1 1 calc R U .
H14B H 0.4038 0.6622 0.6955 0.102 Uiso 1 1 calc R U .
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'
I I -0.4742 1.8119 '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
Cu1 I1 Cu2 59.43(3) . .
Cu1 I1 Cu1 57.86(3) . 3_565
Cu2 I1 Cu1 57.89(3) . 3_565
Cu1 I2 Cu1 58.78(3) 3_565 2_665
Cu1 I2 Cu1 58.78(3) 3_565 .
Cu1 I2 Cu1 58.78(3) 2_665 .
N1 Cu1 Cu1 139.79(13) . 2_665
N1 Cu1 Cu1 153.98(14) . 3_565
Cu1 Cu1 Cu1 59.998(1) 2_665 3_565
N1 Cu1 Cu2 138.79(13) . .
Cu1 Cu1 Cu2 60.211(18) 2_665 .
Cu1 Cu1 Cu2 60.210(18) 3_565 .
N1 Cu1 I1 106.78(12) . .
Cu1 Cu1 I1 112.18(3) 2_665 .
Cu1 Cu1 I1 63.48(3) 3_565 .
Cu2 Cu1 I1 60.935(19) . .
N1 Cu1 I2 109.94(13) . .
Cu1 Cu1 I2 60.608(15) 2_665 .
Cu1 Cu1 I2 60.608(15) 3_565 .
Cu2 Cu1 I2 110.47(3) . .
I1 Cu1 I2 116.30(3) . .
N1 Cu1 I1 97.76(14) . 2_665
Cu1 Cu1 I1 58.66(3) 2_665 2_665
Cu1 Cu1 I1 108.26(3) 3_565 2_665
Cu2 Cu1 I1 59.31(2) . 2_665
I1 Cu1 I1 112.16(3) . 2_665
I2 Cu1 I1 112.14(3) . 2_665
N2 Cu2 Cu1 144.99(2) . 3_565
N2 Cu2 Cu1 144.99(2) . 2_665
Cu1 Cu2 Cu1 59.58(4) 3_565 2_665
N2 Cu2 Cu1 144.99(2) . .
Cu1 Cu2 Cu1 59.58(4) 3_565 .
Cu1 Cu2 Cu1 59.58(4) 2_665 .
N2 Cu2 I1 104.41(3) . .
Cu1 Cu2 I1 62.79(3) 3_565 .
Cu1 Cu2 I1 110.55(5) 2_665 .
Cu1 Cu2 I1 59.64(2) . .
N2 Cu2 I1 104.41(3) . 3_565
Cu1 Cu2 I1 59.64(2) 3_565 3_565
Cu1 Cu2 I1 62.80(3) 2_665 3_565
Cu1 Cu2 I1 110.55(5) . 3_565
I1 Cu2 I1 114.02(2) . 3_565
N2 Cu2 I1 104.41(3) . 2_665
Cu1 Cu2 I1 110.55(5) 3_565 2_665
Cu1 Cu2 I1 59.64(2) 2_665 2_665
Cu1 Cu2 I1 62.80(3) . 2_665
I1 Cu2 I1 114.02(2) . 2_665
I1 Cu2 I1 114.02(2) 3_565 2_665
O3 Cu3 O3 89.8(2) 8_556 5_554
O3 Cu3 O1 89.02(14) 8_556 .
O3 Cu3 O1 167.58(15) 5_554 .
O3 Cu3 O1 167.57(15) 8_556 10_556
O3 Cu3 O1 89.02(14) 5_554 10_556
O1 Cu3 O1 89.45(19) . 10_556
O3 Cu3 O5 96.49(17) 8_556 .
O3 Cu3 O5 96.49(17) 5_554 .
O1 Cu3 O5 95.93(16) . .
O1 Cu3 O5 95.93(16) 10_556 .
O3 Cu3 Cu4 84.11(11) 8_556 .
O3 Cu3 Cu4 84.11(11) 5_554 .
O1 Cu3 Cu4 83.46(10) . .
O1 Cu3 Cu4 83.46(10) 10_556 .
O5 Cu3 Cu4 179.14(18) . .
O4 Cu4 O4 89.8(2) 5_554 8_556
O4 Cu4 O2 89.69(17) 5_554 10_556
O4 Cu4 O2 167.92(16) 8_556 10_556
O4 Cu4 O2 167.93(16) 5_554 .
O4 Cu4 O2 89.69(17) 8_556 .
O2 Cu4 O2 88.3(2) 10_556 .
O4 Cu4 O6 98.58(17) 5_554 .
O4 Cu4 O6 98.58(17) 8_556 .
O2 Cu4 O6 93.43(16) 10_556 .
O2 Cu4 O6 93.42(16) . .
O4 Cu4 Cu3 83.65(12) 5_554 .
O4 Cu4 Cu3 83.65(12) 8_556 .
O2 Cu4 Cu3 84.31(10) 10_556 .
O2 Cu4 Cu3 84.31(10) . .
O6 Cu4 Cu3 176.83(17) . .
C6 O1 Cu3 122.4(3) . .
C6 O2 Cu4 123.2(3) . .
C13 O3 Cu3 121.2(3) . 9_556
C13 O4 Cu4 124.0(4) . 9_556
C5 N1 C1 115.8(5) . .
C5 N1 Cu1 121.0(4) . .
C1 N1 Cu1 122.8(3) . .
C14 N2 C14 108.0(4) 2_665 3_565
C14 N2 C14 108.0(4) 2_665 .
C14 N2 C14 108.0(4) 3_565 .
C14 N2 Cu2 110.9(4) 2_665 .
C14 N2 Cu2 110.9(4) 3_565 .
C14 N2 Cu2 110.9(4) . .
N1 C1 C2 123.9(5) . .
N1 C1 H1 118.1 . .
C2 C1 H1 118.1 . .
C3 C2 C1 118.9(4) . .
C3 C2 C6 123.0(5) . .
C1 C2 C6 118.1(4) . .
C2 C3 C4 118.7(5) . .
C2 C3 H3 120.7 . .
C4 C3 H3 120.7 . .
C5 C4 C3 117.8(5) . .
C5 C4 C7 118.3(5) . .
C3 C4 C7 123.8(5) . .
N1 C5 C4 125.0(5) . .
N1 C5 H5 117.5 . .
C4 C5 H5 117.5 . .
O1 C6 O2 126.7(4) . .
O1 C6 C2 118.2(4) . .
O2 C6 C2 115.1(5) . .
C8 C7 C12 119.5(5) . .
C8 C7 C4 119.5(5) . .
C12 C7 C4 120.9(5) . .
C7 C8 C9 119.1(6) . .
C7 C8 H8 120.5 . .
C9 C8 H8 120.5 . .
C10 C9 C8 121.1(5) . .
C10 C9 H9 119.5 . .
C8 C9 H9 119.5 . .
C11 C10 C9 118.8(5) . .
C11 C10 C13 119.8(5) . .
C9 C10 C13 121.3(5) . .
C10 C11 C12 119.7(6) . .
C10 C11 H11 120.1 . .
C12 C11 H11 120.1 . .
C7 C12 C11 121.6(6) . .
C7 C12 H12 119.2 . .
C11 C12 H12 119.2 . .
O4 C13 O3 127.1(5) . .
O4 C13 C10 114.5(5) . .
O3 C13 C10 118.5(5) . .
N2 C14 C14 110.9(4) . 10_557
N2 C14 H14A 109.5 . .
C14 C14 H14A 109.5 10_557 .
N2 C14 H14B 109.5 . .
C14 C14 H14B 109.5 10_557 .
H14A C14 H14B 108.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Cu1 2.6567(8) .
I1 Cu2 2.6913(6) .
I1 Cu1 2.7834(10) 3_565
I2 Cu1 2.6837(10) 3_565
I2 Cu1 2.6837(10) 2_665
I2 Cu1 2.6837(10) .
Cu1 N1 2.020(4) .
Cu1 Cu1 2.6341(13) 2_665
Cu1 Cu1 2.6341(12) 3_565
Cu1 Cu2 2.6510(13) .
Cu1 I1 2.7834(10) 2_665
Cu2 N2 2.071(8) .
Cu2 Cu1 2.6510(13) 3_565
Cu2 Cu1 2.6510(13) 2_665
Cu2 I1 2.6913(6) 3_565
Cu2 I1 2.6913(6) 2_665
Cu3 O3 1.969(3) 8_556
Cu3 O3 1.969(3) 5_554
Cu3 O1 1.998(3) .
Cu3 O1 1.998(3) 10_556
Cu3 O5 2.126(6) .
Cu3 Cu4 2.6545(12) .
Cu4 O4 1.932(3) 5_554
Cu4 O4 1.932(3) 8_556
Cu4 O2 1.954(3) 10_556
Cu4 O2 1.954(3) .
Cu4 O6 2.221(6) .
O1 C6 1.239(5) .
O2 C6 1.261(5) .
O3 C13 1.259(6) .
O3 Cu3 1.969(3) 9_556
O4 C13 1.242(6) .
O4 Cu4 1.932(3) 9_556
N1 C5 1.341(6) .
N1 C1 1.345(6) .
N2 C14 1.473(6) 2_665
N2 C14 1.473(6) 3_565
N2 C14 1.473(6) .
C1 C2 1.389(7) .
C1 H1 0.9300 .
C2 C3 1.379(6) .
C2 C6 1.490(6) .
C3 C4 1.396(7) .
C3 H3 0.9300 .
C4 C5 1.383(7) .
C4 C7 1.495(7) .
C5 H5 0.9300 .
C7 C8 1.373(8) .
C7 C12 1.382(7) .
C8 C9 1.411(7) .
C8 H8 0.9300 .
C9 C10 1.393(7) .
C9 H9 0.9300 .
C10 C11 1.377(7) .
C10 C13 1.517(7) .
C11 C12 1.390(7) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C14 C14 1.550(10) 10_557
C14 H14A 0.9700 .
C14 H14B 0.9700 .
