#------------------------------------------------------------------------------
#$Date: 2019-09-10 02:59:18 +0300 (Tue, 10 Sep 2019) $
#$Revision: 218104 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/41/7124136.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_7124136
loop_
_publ_author_name
'Lama, Prem'
'Hazra, Arpan'
'Barbour, Len'
_publ_section_title
;
 Accordion and layer-sliding motion to produce anomalous thermal expansion
 behaviour in 2D-coordination polymers
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC06634A
_journal_year                    2019
_chemical_formula_sum            'C32 H29 N3 O9 Zn2'
_chemical_formula_weight         730.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-08-14 deposited with the CCDC.    2019-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.248(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.3338(2)
_cell_length_b                   21.5667(5)
_cell_length_c                   9.4299(2)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      25.93
_cell_measurement_theta_min      2.29
_cell_volume                     1600.12(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 venture PHOTON II CPAD'
_diffrn_measurement_method       'φ \ch and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            49288
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         2.288
_exptl_absorpt_coefficient_mu    1.557
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.496
_exptl_crystal_size_mid          0.378
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0436P)²+6.1363P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1225
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2637
_reflns_number_total             2887
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc06634a3.cif
_cod_data_source_block           2_160K
_cod_database_code               7124136
_shelx_shelxl_version_number     2016/6
_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_min   0.512
_shelx_estimated_absorpt_t_max   0.921
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.35933(4) 0.50093(2) 0.60622(3) 0.02357(8) Uani 1 1 d . . . . .
O1 O 0.3378(3) 0.58976(10) 0.5930(2) 0.0359(6) Uani 1 1 d . . . . .
O2 O 0.3947(3) 0.58557(11) 0.8391(2) 0.0417(6) Uani 1 1 d . . . . .
O3 O 0.2460(2) 0.47401(10) 0.39488(19) 0.0276(5) Uani 1 1 d . . . . .
O4 O 0.4079(2) 0.52733(10) 0.2917(2) 0.0282(5) Uani 1 1 d . . . . .
O5 O 0.439360 0.741301 0.223560 0.245(6) Uiso 0.5 1 d . . P A -1
N1 N 0.2339(3) 0.44581(11) 0.7043(2) 0.0253(5) Uani 1 1 d . . . . .
N2 N 0.680620 0.728520 0.442889 0.113(4) Uiso 0.5 1 d . . P A -1
C1 C 0.3646(4) 0.61553(14) 0.7225(3) 0.0308(7) Uani 1 1 d . . . . .
C2 C 0.3620(4) 0.68492(14) 0.7235(3) 0.0290(7) Uani 1 1 d . . . . .
C3 C 0.3741(4) 0.71779(15) 0.8542(3) 0.0360(8) Uani 1 1 d . . . . .
H3 H 0.382489 0.695938 0.943799 0.043 Uiso 1 1 calc R U . . .
C4 C 0.3493(4) 0.71814(15) 0.5921(3) 0.0340(8) Uani 1 1 d . . . . .
H4 H 0.340576 0.696338 0.502311 0.041 Uiso 1 1 calc R U . . .
C5 C 0.2719(3) 0.50018(12) 0.2855(3) 0.0234(6) Uani 1 1 d . . . . .
C6 C 0.1309(3) 0.49996(12) 0.1374(3) 0.0223(6) Uani 1 1 d . . . . .
C7 C 0.1472(3) 0.53431(13) 0.0172(3) 0.0244(6) Uani 1 1 d . . . . .
H7 H 0.247638 0.557488 0.028887 0.029 Uiso 1 1 calc R U . . .
C8 C -0.0161(3) 0.46559(13) 0.1190(3) 0.0234(6) Uani 1 1 d . . . . .
H8 H -0.026529 0.441905 0.200446 0.028 Uiso 1 1 calc R U . . .
C9 C 0.3093(4) 0.42728(14) 0.8475(3) 0.0290(7) Uani 1 1 d . . . . .
H9 H 0.417663 0.443766 0.902616 0.035 Uiso 1 1 calc R U . . .
C10 C 0.2350(4) 0.38537(15) 0.9165(3) 0.0349(8) Uani 1 1 d . . . . .
H10 H 0.293054 0.372682 1.016865 0.042 Uiso 1 1 calc R U . . .
C11 C 0.0757(4) 0.36167(14) 0.8399(3) 0.0351(7) Uani 1 1 d . . . . .
C12 C -0.0039(4) 0.38217(15) 0.6941(3) 0.0351(8) Uani 1 1 d . . . . .
H12 H -0.114768 0.367907 0.638694 0.042 Uiso 1 1 calc R U . . .
C13 C 0.0784(3) 0.42327(14) 0.6301(3) 0.0299(7) Uani 1 1 d . . . . .
H13 H 0.023226 0.436219 0.529477 0.036 Uiso 1 1 calc R U . . .
C14 C 0.0000(4) 0.31023(16) 0.9042(4) 0.0446(9) Uani 1 1 d . . . . .
H14A H -0.125699 0.312546 0.866103 0.054 Uiso 1 1 calc R U . . .
H14B H 0.039131 0.312653 1.015194 0.054 Uiso 1 1 calc R U . . .
C15 C 0.0615(7) 0.250000 0.8526(6) 0.0484(13) Uani 1 2 d S T P . .
H15A H 0.024134 0.250000 0.741432 0.058 Uiso 1 2 calc R U P . .
H15B H 0.187313 0.250000 0.889506 0.058 Uiso 1 2 calc R U P . .
C16 C 0.544909 0.710110 0.315620 0.127(5) Uiso 0.5 1 d . . P A -1
H16 H 0.534218 0.666621 0.299198 0.152 Uiso 0.5 1 calc R U P A -1
C17 C 0.792700 0.697050 0.568841 0.121(5) Uiso 0.5 1 d . . P A -1
H17A H 0.743252 0.656989 0.580962 0.182 Uiso 0.5 1 calc R U P A -1
H17B H 0.810332 0.722144 0.659361 0.182 Uiso 0.5 1 calc R U P A -1
H17C H 0.901945 0.690277 0.553212 0.182 Uiso 0.5 1 calc R U P A -1
C18 C 0.698791 0.793620 0.450049 0.158(7) Uiso 0.5 1 d . . P A -1
H18A H 0.789396 0.805840 0.410840 0.237 Uiso 0.5 1 calc R U P A -1
H18B H 0.727899 0.807238 0.554657 0.237 Uiso 0.5 1 calc R U P A -1
H18C H 0.591694 0.812985 0.389623 0.237 Uiso 0.5 1 calc R U P A -1
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'
Zn Zn 0.2839 1.4301 '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
O1 Zn1 O4 113.46(9) . 3_666
O1 Zn1 O3 102.84(8) . .
O4 Zn1 O3 117.90(8) 3_666 .
O1 Zn1 N1 124.74(10) . .
O4 Zn1 N1 99.90(9) 3_666 .
O3 Zn1 N1 98.17(8) . .
C1 O1 Zn1 112.57(18) . .
C5 O3 Zn1 122.57(17) . .
C5 O4 Zn1 127.49(18) . 3_666
C13 N1 C9 117.7(3) . .
C13 N1 Zn1 122.37(18) . .
C9 N1 Zn1 119.81(19) . .
C16 N2 C18 111.389(1) . .
C16 N2 C17 134.504(2) . .
C18 N2 C17 113.907(2) . .
O2 C1 O1 122.7(3) . .
O2 C1 C2 121.3(3) . .
O1 C1 C2 116.0(2) . .
C3 C2 C4 118.8(3) . .
C3 C2 C1 121.1(3) . .
C4 C2 C1 120.1(3) . .
C3 C3 C2 120.52(18) 4_575 .
C3 C3 H3 119.7 4_575 .
C2 C3 H3 119.7 . .
C4 C4 C2 120.67(18) 4_575 .
C4 C4 H4 119.7 4_575 .
C2 C4 H4 119.7 . .
O3 C5 O4 124.5(2) . .
O3 C5 C6 118.0(2) . .
O4 C5 C6 117.4(2) . .
C8 C6 C7 119.8(2) . .
C8 C6 C5 120.3(2) . .
C7 C6 C5 119.9(2) . .
C8 C7 C6 119.7(2) 3_565 .
C8 C7 H7 120.1 3_565 .
C6 C7 H7 120.1 . .
C7 C8 C6 120.5(2) 3_565 .
C7 C8 H8 119.8 3_565 .
C6 C8 H8 119.8 . .
N1 C9 C10 122.3(3) . .
N1 C9 H9 118.8 . .
C10 C9 H9 118.8 . .
C9 C10 C11 120.0(3) . .
C9 C10 H10 120.0 . .
C11 C10 H10 120.0 . .
C10 C11 C12 117.6(3) . .
C10 C11 C14 121.5(3) . .
C12 C11 C14 120.6(3) . .
C13 C12 C11 119.7(3) . .
C13 C12 H12 120.2 . .
C11 C12 H12 120.2 . .
N1 C13 C12 122.6(3) . .
N1 C13 H13 118.7 . .
C12 C13 H13 118.7 . .
C11 C14 C15 105.6(3) . .
C11 C14 H14A 110.6 . .
C15 C14 H14A 110.6 . .
C11 C14 H14B 110.6 . .
C15 C14 H14B 110.6 . .
H14A C14 H14B 108.7 . .
C14 C15 C14 115.8(4) 4_565 .
C14 C15 H15A 108.3 4_565 .
C14 C15 H15A 108.3 . .
C14 C15 H15B 108.3 4_565 .
C14 C15 H15B 108.3 . .
H15A C15 H15B 107.4 . .
O5 C16 N2 129.926(1) . .
O5 C16 H16 115.0 . .
N2 C16 H16 115.0 . .
N2 C17 H17A 109.5 . .
N2 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
N2 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
N2 C18 H18A 109.5 . .
N2 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
N2 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.924(2) .
Zn1 O4 1.9572(18) 3_666
Zn1 O3 1.9899(17) .
Zn1 N1 2.000(2) .
O1 C1 1.292(4) .
O2 C1 1.228(4) .
O3 C5 1.255(3) .
O4 C5 1.260(3) .
O5 C16 1.215078(18) .
N1 C13 1.344(3) .
N1 C9 1.348(3) .
N2 C16 1.40790(3) .
N2 C18 1.41136(3) .
N2 C17 1.41856(3) .
C1 C2 1.497(4) .
C2 C3 1.396(4) .
C2 C4 1.405(4) .
C3 C3 1.389(7) 4_575
C3 H3 0.9500 .
C4 C4 1.374(6) 4_575
C4 H4 0.9500 .
C5 C6 1.500(3) .
C6 C8 1.393(4) .
C6 C7 1.397(4) .
C7 C8 1.385(3) 3_565
C7 H7 0.9500 .
C8 H8 0.9500 .
C9 C10 1.375(4) .
C9 H9 0.9500 .
C10 C11 1.383(4) .
C10 H10 0.9500 .
C11 C12 1.388(4) .
C11 C14 1.499(5) .
C12 C13 1.376(5) .
C12 H12 0.9500 .
C13 H13 0.9500 .
C14 C15 1.533(5) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 H16 0.9500 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
