#------------------------------------------------------------------------------
#$Date: 2016-03-22 13:53:46 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178981 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/04/4120432.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_4120432
loop_
_publ_author_name
'Murdock, Christopher R.'
'McNutt, Nicholas W.'
'Keffer, David J.'
'Jenkins, David M.'
_publ_section_title
;
 Rotating phenyl rings as a guest-dependent switch in two-dimensional
 metal-organic frameworks.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              671
_journal_page_last               678
_journal_paper_doi               10.1021/ja4088709
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C15 H19 Cl Cu N7 O6'
_chemical_formula_weight         492.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 126.334(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.381(9)
_cell_length_b                   7.616(4)
_cell_length_c                   15.488(7)
_cell_measurement_temperature    100(2)
_cell_volume                     2031.7(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0894
_diffrn_reflns_av_sigmaI/netI    0.0838
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8338
_diffrn_reflns_theta_full        24.90
_diffrn_reflns_theta_max         24.90
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.758
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         1889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1007P)²+1.2423P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1623
_refine_ls_wR_factor_ref         0.1884
_reflns_number_gt                1243
_reflns_number_total             1889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4088709_si_002.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'c 2/m'
_cod_database_code               4120432
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.5000 0.24817(14) 0.5000 0.0331(4) Uani 1 2 d S
Cl1 Cl 0.38029(13) 0.0000 0.08156(15) 0.0406(6) Uani 1 2 d S
N2 N 0.3028(4) 0.0000 0.2444(5) 0.042(2) Uani 1 2 d S
N1 N 0.4087(3) 0.0904(6) 0.3967(3) 0.0350(12) Uani 1 1 d .
N4 N 0.4749(4) 0.5000 0.2438(4) 0.0323(17) Uani 1 2 d S
N3 N 0.5023(3) 0.4096(6) 0.3966(3) 0.0326(12) Uani 1 1 d .
C7 C 0.5281(5) 0.5000 0.1392(5) 0.032(2) Uani 1 2 d S
C1 C 0.3442(4) 0.1375(10) 0.3037(4) 0.0455(17) Uani 1 1 d .
H1 H 0.3296 0.2535 0.2824 0.055 Uiso 1 1 calc R
C4 C 0.1265(4) 0.1562(11) 0.1399(4) 0.0470(18) Uani 1 1 d .
H4 H 0.1483 0.2620 0.1401 0.056 Uiso 1 1 calc R
C5 C 0.4863(3) 0.3600(8) 0.3041(4) 0.0302(14) Uani 1 1 d .
H5 H 0.4833 0.2439 0.2834 0.036 Uiso 1 1 calc R
C6 C 0.4551(4) 0.5000 0.1336(5) 0.033(2) Uani 1 2 d S
H6A H 0.4244 0.6031 0.0950 0.040 Uiso 0.50 1 calc PR
H6B H 0.4244 0.3969 0.0950 0.040 Uiso 0.50 1 calc PR
C3 C 0.1598(5) 0.0000 0.1403(5) 0.036(2) Uani 1 2 d S
C2 C 0.2278(5) 0.0000 0.1356(6) 0.056(3) Uani 1 2 d S
H2A H 0.2252 -0.1030 0.0967 0.068 Uiso 0.50 1 calc PR
H2B H 0.2252 0.1030 0.0967 0.068 Uiso 0.50 1 calc PR
C8 C 0.5612(3) 0.6584(9) 0.1394(4) 0.0404(16) Uani 1 1 d .
H8 H 0.5397 0.7647 0.1391 0.049 Uiso 1 1 calc R
C11 C 0.2816(8) 0.5000 0.5818(8) 0.100(5) Uani 1 2 d S
H11A H 0.2462 0.5000 0.6008 0.150 Uiso 1 2 calc SR
H11B H 0.3137 0.6029 0.6106 0.150 Uiso 0.50 1 calc PR
H11C H 0.3137 0.3971 0.6106 0.150 Uiso 0.50 1 calc PR
C9 C 0.2747(9) 0.5000 0.4204(12) 0.081(4) Uani 1 2 d S
H9 H 0.3287 0.5000 0.4668 0.097 Uiso 1 2 calc SR
C10 C 0.1554(7) 0.5000 0.4067(10) 0.099(5) Uani 1 2 d S
H10A H 0.1422 0.5000 0.4561 0.149 Uiso 1 2 calc SR
H10B H 0.1343 0.3971 0.3625 0.149 Uiso 0.50 1 calc PR
H10C H 0.1343 0.6029 0.3625 0.149 Uiso 0.50 1 calc PR
N5 N 0.2375(5) 0.5000 0.4647(6) 0.051(2) Uani 1 2 d S
O1 O 0.2457(8) 0.5000 0.3263(9) 0.121(4) Uani 1 2 d S
O3 O 0.4570(4) 0.0000 0.1824(5) 0.0556(18) Uani 1 2 d S
O2 O 0.3404(3) 0.1542(7) 0.0762(4) 0.0682(15) Uani 1 1 d .
O4 O 0.3935(7) 0.0000 0.0023(6) 0.107(4) Uani 1 2 d S
O5 O 0.2878(8) 0.5000 0.1910(11) 0.179(6) Uani 1 2 d S
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'
Cl Cl 0.1484 0.1585 '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
N1 Cu1 N1 107.3(3) . 2_656
N1 Cu1 N3 121.04(18) . 2_656
N1 Cu1 N3 101.38(17) 2_656 2_656
N1 Cu1 N3 101.38(17) . .
N1 Cu1 N3 121.04(18) 2_656 .
N3 Cu1 N3 106.0(3) 2_656 .
O4 Cl1 O2 111.7(3) . 6
O4 Cl1 O2 111.7(3) . .
O2 Cl1 O2 111.0(4) 6 .
O4 Cl1 O3 104.8(6) . .
O2 Cl1 O3 108.6(3) 6 .
O2 Cl1 O3 108.6(3) . .
C1 N2 C1 104.3(7) . 6
C1 N2 C2 127.9(3) . .
C1 N2 C2 127.9(3) 6 .
C1 N1 N1 105.7(4) . 6
C1 N1 Cu1 126.4(5) . .
N1 N1 Cu1 126.33(13) 6 .
C5 N4 C5 105.2(6) 6_565 .
C5 N4 C6 127.4(3) 6_565 .
C5 N4 C6 127.4(3) . .
C5 N3 N3 106.7(3) . 6_565
C5 N3 Cu1 124.7(4) . .
N3 N3 Cu1 127.00(13) 6_565 .
C8 C7 C8 119.3(8) 6_565 .
C8 C7 C6 120.3(4) 6_565 .
C8 C7 C6 120.3(4) . .
N1 C1 N2 112.1(6) . .
N1 C1 H1 123.9 . .
N2 C1 H1 123.9 . .
C3 C4 C8 121.5(7) . 3_445
C3 C4 H4 119.3 . .
C8 C4 H4 119.3 3_445 .
N3 C5 N4 110.7(5) . .
N3 C5 H5 124.7 . .
N4 C5 H5 124.7 . .
N4 C6 C7 110.5(6) . .
N4 C6 H6A 109.5 . .
C7 C6 H6A 109.5 . .
N4 C6 H6B 109.5 . .
C7 C6 H6B 109.5 . .
H6A C6 H6B 108.1 . .
C4 C3 C4 118.4(8) 6 .
C4 C3 C2 120.7(4) 6 .
C4 C3 C2 120.7(4) . .
N2 C2 C3 111.8(6) . .
N2 C2 H2A 109.3 . .
C3 C2 H2A 109.3 . .
N2 C2 H2B 109.3 . .
C3 C2 H2B 109.3 . .
H2A C2 H2B 107.9 . .
C4 C8 C7 119.7(7) 3 .
C4 C8 H8 120.2 3 .
C7 C8 H8 120.2 . .
N5 C11 H11A 109.5 . .
N5 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
N5 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
O1 C9 N5 126.4(15) . .
O1 C9 H9 116.8 . .
N5 C9 H9 116.8 . .
N5 C10 H10A 109.5 . .
N5 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
N5 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C9 N5 C10 124.7(11) . .
C9 N5 C11 119.9(11) . .
C10 N5 C11 115.4(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 2.028(5) .
Cu1 N1 2.028(5) 2_656
Cu1 N3 2.043(4) 2_656
Cu1 N3 2.043(4) .
Cl1 O4 1.415(7) .
Cl1 O2 1.425(5) 6
Cl1 O2 1.425(5) .
Cl1 O3 1.447(6) .
N2 C1 1.327(8) .
N2 C1 1.327(8) 6
N2 C2 1.487(9) .
N1 C1 1.324(7) .
N1 N1 1.377(10) 6
N4 C5 1.342(6) 6_565
N4 C5 1.342(6) .
N4 C6 1.494(8) .
N3 C5 1.315(6) .
N3 N3 1.377(9) 6_565
C7 C8 1.398(8) 6_565
C7 C8 1.398(8) .
C7 C6 1.512(11) .
C1 H1 0.9300 .
C4 C3 1.385(9) .
C4 C8 1.390(9) 3_445
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C3 C4 1.385(9) 6
C3 C2 1.498(12) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C8 C4 1.390(9) 3
C8 H8 0.9300 .
C11 N5 1.467(13) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C9 O1 1.199(15) .
C9 N5 1.324(15) .
C9 H9 0.9300 .
C10 N5 1.421(14) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
