#------------------------------------------------------------------------------
#$Date: 2017-01-01 03:26:02 +0200 (Sun, 01 Jan 2017) $
#$Revision: 189527 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/49/4344929.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_4344929
loop_
_publ_author_name
'Maity, Dilip Kumar'
'Halder, Arijit'
'Pahari, Goutam'
'Haque, Fazle'
'Ghoshal, Debajyoti'
_publ_section_title
;
 Hydrogen Uptake by an Inclined Polycatenated Dynamic Metal-Organic
 Framework Based Material.
;
_journal_name_full               'Inorganic chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.6b02719
_journal_year                    2016
_chemical_formula_sum            'C20 H21 Cu N3 O10'
_chemical_formula_weight         526.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_symmetry_space_group_name_Hall  'I -2ya'
_symmetry_space_group_name_H-M   'I 1 a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 103.198(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   12.743(5)
_cell_length_b                   10.874(5)
_cell_length_c                   17.709(5)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      2.2
_cell_volume                     2389.1(16)
_computing_cell_refinement       'SMART APEX II'
_computing_data_collection       'SMART APEX II (BRUKER,2010)'
_computing_data_reduction        'SAINT (BRUKER,2000)'
_computing_molecular_graphics    'Ortep-3v2 for windows (Farrugia,1997)'
_computing_publication_material  'PLATON (Spek, 2008)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17958
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.577
_diffrn_reflns_theta_min         2.214
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_T_max  0.9852
_exptl_absorpt_correction_T_min  0.8859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'XPREP' - A PROGRAM DATA PREPARATION & RECIPROCAL 
SPACE EXPLORATION,
Bruker Analytical X-ray Systems, 1997
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       Linear
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.31(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5389
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0512
_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)+(0.0661P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1268
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                3993
_reflns_number_total             5389
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02719_si_002.cif
_cod_data_source_block           DG1_rev
_cod_database_code               4344929
_shelx_shelxl_version_number     2016/4
_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'
'x+1/2, -y, z'
'x+1/2, y+1/2, z+1/2'
'x+1, -y+1/2, 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
CU1 Cu 0.04674(6) 0.22877(7) 0.39681(5) 0.0440(3) Uani 1 1 d . .
O2 O 0.2485(5) 0.2702(5) 0.5343(4) 0.0639(15) Uani 1 1 d . .
O1 O 0.1357(4) 0.1224(4) 0.4759(3) 0.0455(12) Uani 1 1 d . .
C5 C 0.1299(7) 0.2041(8) 0.2578(5) 0.052(2) Uani 1 1 d . .
H5 H 0.122661 0.289227 0.256854 0.062 Uiso 1 1 calc R U
C14 C 0.2528(5) 0.0788(6) 0.5967(4) 0.0362(15) Uani 1 1 d . .
N1 N 0.1020(4) 0.1411(6) 0.3140(3) 0.0375(14) Uani 1 1 d . .
C18 C 0.3931(6) 0.0143(6) 0.7071(4) 0.0405(15) Uani 1 1 d . .
H18 H 0.463534 0.022426 0.735861 0.049 Uiso 1 1 calc R U
C19 C 0.3557(5) 0.0861(6) 0.6420(4) 0.0383(16) Uani 1 1 d . .
C15 C 0.1861(6) -0.0049(7) 0.6191(4) 0.052(2) Uani 1 1 d . .
H15 H 0.116182 -0.013739 0.589466 0.063 Uiso 1 1 calc R U
C2 C 0.1443(6) -0.0421(7) 0.2559(4) 0.0494(18) Uani 1 1 d . .
H2 H 0.146185 -0.127586 0.256613 0.059 Uiso 1 1 calc R U
C6 C 0.2220(5) -0.0415(8) 0.1349(5) 0.052(2) Uani 1 1 d . .
H6A H 0.196697 -0.125782 0.127875 0.062 Uiso 1 1 calc R U
H6B H 0.196031 0.001983 0.086438 0.062 Uiso 1 1 calc R U
C4 C 0.1692(6) 0.1472(7) 0.2006(4) 0.055(2) Uani 1 1 d . .
H4 H 0.190733 0.194237 0.162995 0.066 Uiso 1 1 calc R U
C13 C 0.2105(5) 0.1652(7) 0.5286(4) 0.0420(16) Uani 1 1 d . .
O5 O 0.4782(7) 0.2453(7) 0.6663(7) 0.132(4) Uani 1 1 d . .
N3 N 0.4350(6) 0.1701(8) 0.6189(6) 0.075(2) Uani 1 1 d . .
C1 C 0.1086(5) 0.0193(7) 0.3129(4) 0.0429(17) Uani 1 1 d . .
H1 H 0.088400 -0.025754 0.351886 0.051 Uiso 1 1 calc R U
O6 O 0.4514(6) 0.1529(9) 0.5539(6) 0.126(4) Uani 1 1 d . .
C3 C 0.1770(5) 0.0192(7) 0.1987(4) 0.0445(17) Uani 1 1 d . .
C7 C -0.1565(6) 0.4600(9) 0.6557(5) 0.059(2) Uani 1 1 d . .
H7A H -0.131865 0.544319 0.664742 0.071 Uiso 1 1 calc R U
H7B H -0.131147 0.414707 0.703612 0.071 Uiso 1 1 calc R U
C12 C -0.0696(6) 0.4779(7) 0.5430(4) 0.0458(17) Uani 1 1 d . .
H12 H -0.073123 0.563079 0.546566 0.055 Uiso 1 1 calc R U
C9 C -0.1029(6) 0.2802(7) 0.5829(5) 0.057(2) Uani 1 1 d . .
H9 H -0.130009 0.226539 0.614664 0.068 Uiso 1 1 calc R U
C8 C -0.1084(5) 0.4052(7) 0.5940(4) 0.0472(18) Uani 1 1 d . .
C17 C 0.3242(5) -0.0693(6) 0.7286(4) 0.0356(14) Uani 1 1 d . .
C16 C 0.2197(6) -0.0783(6) 0.6858(4) 0.052(2) Uani 1 1 d . .
H16 H 0.171777 -0.132485 0.700786 0.063 Uiso 1 1 calc R U
C11 C -0.0253(5) 0.4252(7) 0.4866(4) 0.0439(17) Uani 1 1 d . .
H11 H 0.000813 0.476250 0.452947 0.053 Uiso 1 1 calc R U
C10 C -0.0583(8) 0.2345(7) 0.5262(6) 0.051(2) Uani 1 1 d . .
H10 H -0.055431 0.149585 0.520612 0.061 Uiso 1 1 calc R U
N2 N -0.0186(4) 0.3049(5) 0.4785(3) 0.0396(14) Uani 1 1 d . .
O1W O 0.2042(4) 0.3865(4) 0.3968(3) 0.091(2) Uani 1 1 d G .
H1WA H 0.218887 0.348812 0.439927 0.136 Uiso 1 1 d G U
H1WB H 0.181518 0.458380 0.403269 0.136 Uiso 1 1 d G U
O2W O -0.1031(4) 0.0568(5) 0.3820(4) 0.090(2) Uani 1 1 d G .
H2WA H -0.082005 0.041148 0.430088 0.135 Uiso 1 1 d G U
H2WB H -0.090468 -0.004633 0.355774 0.135 Uiso 1 1 d G U
O3W O 0.1266(6) 0.6230(4) 0.3693(6) 0.160(4) Uani 1 1 d G .
H3WA H 0.131169 0.635577 0.322799 0.240 Uiso 1 1 d G U
H3WB H 0.174112 0.665451 0.399873 0.240 Uiso 1 1 d G U
O4W O 0.4081(5) 0.2422(6) 0.3706(8) 0.234(7) Uani 1 1 d G .
O4 O 0.2997(5) -0.2243(5) 0.8172(4) 0.0705(18) Uani 1 1 d . .
C20 C 0.3647(5) -0.1584(6) 0.7938(4) 0.0393(15) Uani 1 1 d . .
O3 O 0.4658(4) -0.1591(4) 0.8185(3) 0.0447(12) 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 0.0033 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'
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
O3 CU1 O1 176.6(2) 3_454 .
O3 CU1 N1 89.7(2) 3_454 .
O1 CU1 N1 90.0(2) . .
O3 CU1 N2 90.9(2) 3_454 .
O1 CU1 N2 89.8(2) . .
N1 CU1 N2 174.9(2) . .
C13 O1 CU1 121.7(5) . .
N1 C5 C4 121.8(7) . .
C15 C14 C19 116.3(6) . .
C15 C14 C13 120.6(6) . .
C19 C14 C13 122.9(6) . .
C5 N1 C1 118.5(6) . .
C5 N1 CU1 120.2(5) . .
C1 N1 CU1 121.3(5) . .
C17 C18 C19 118.9(6) . .
C14 C19 C18 123.7(6) . .
C14 C19 N3 119.5(6) . .
C18 C19 N3 116.8(6) . .
C14 C15 C16 122.1(6) . .
C3 C2 C1 121.4(7) . .
C7 C6 C3 110.6(5) 3_544 .
C5 C4 C3 120.5(7) . .
O2 C13 O1 128.1(7) . .
O2 C13 C14 116.3(6) . .
O1 C13 C14 115.4(6) . .
O5 N3 O6 127.1(10) . .
O5 N3 C19 117.0(10) . .
O6 N3 C19 115.8(9) . .
N1 C1 C2 122.0(7) . .
C2 C3 C4 115.8(6) . .
C2 C3 C6 124.8(7) . .
C4 C3 C6 119.3(7) . .
C8 C7 C6 112.7(6) . 3_455
C8 C12 C11 120.3(7) . .
C10 C9 C8 120.7(8) . .
C12 C8 C9 115.9(7) . .
C12 C8 C7 121.3(8) . .
C9 C8 C7 122.8(8) . .
C16 C17 C18 119.5(6) . .
C16 C17 C20 119.7(6) . .
C18 C17 C20 120.6(6) . .
C17 C16 C15 119.5(7) . .
N2 C11 C12 122.5(7) . .
N2 C10 C9 123.1(7) . .
C10 N2 C11 117.4(6) . .
C10 N2 CU1 120.3(5) . .
C11 N2 CU1 122.3(5) . .
O4 C20 O3 126.0(6) . .
O4 C20 C17 119.5(6) . .
O3 C20 C17 114.5(6) . .
C20 O3 CU1 125.6(4) . 3_545
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
CU1 O3 1.954(4) 3_454
CU1 O1 1.965(4) .
CU1 N1 2.007(5) .
CU1 N2 2.006(5) .
O2 C13 1.236(9) .
O1 C13 1.260(8) .
C5 N1 1.323(11) .
C5 C4 1.375(11) .
C14 C15 1.365(10) .
C14 C19 1.375(9) .
C14 C13 1.526(9) .
N1 C1 1.327(9) .
C18 C17 1.376(9) .
C18 C19 1.383(9) .
C19 N3 1.487(10) .
C15 C16 1.408(9) .
C2 C3 1.356(10) .
C2 C1 1.370(10) .
C6 C7 1.508(9) 3_544
C6 C3 1.527(9) .
C4 C3 1.396(11) .
O5 N3 1.210(12) .
N3 O6 1.231(11) .
C7 C8 1.494(10) .
C7 C6 1.508(9) 3_455
C12 C8 1.375(10) .
C12 C11 1.379(9) .
C9 C10 1.356(12) .
C9 C8 1.377(11) .
C17 C16 1.376(9) .
C17 C20 1.506(8) .
C11 N2 1.321(9) .
C10 N2 1.323(10) .
O4 C20 1.237(9) .
C20 O3 1.262(8) .
O3 CU1 1.954(4) 3_545
