#------------------------------------------------------------------------------
#$Date: 2019-09-10 02:59:18 +0300 (Tue, 10 Sep 2019) $
#$Revision: 218104 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/41/7124134.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_7124134
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                 109.423(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.3674(3)
_cell_length_b                   21.5772(8)
_cell_length_c                   9.4332(3)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      2.58
_cell_volume                     1606.19(10)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0288
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_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       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            29209
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.476
_exptl_absorpt_coefficient_mu    1.551
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.510
_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          0.055
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0302P)²+5.0539P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2777
_reflns_number_total             2881
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc06634a3.cif
_cod_data_source_block           2_200K
_cod_database_code               7124134
_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   0.513
_shelx_estimated_absorpt_t_max   0.920
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 0.35967(3) 0.49894(2) 0.10657(3) 0.02689(8) Uani 1 1 d . . . . .
O1 O 0.3372(3) 0.41017(9) 0.0930(2) 0.0411(6) Uani 1 1 d . . . . .
O2 O 0.3922(3) 0.41440(10) 0.3384(2) 0.0491(6) Uani 1 1 d . . . . .
O3 O 0.5924(2) 0.52689(10) 0.20873(19) 0.0335(5) Uani 1 1 d . . . . .
O4 O 0.7535(2) 0.47409(9) 0.10478(18) 0.0321(5) Uani 1 1 d . . . . .
O5 O 0.440310 0.270909 -0.275591 0.198(5) Uiso 0.5 1 d . . P A -1
N1 N 0.2352(3) 0.55424(11) 0.2047(2) 0.0284(5) Uani 1 1 d . . . . .
N2 N 0.690181 0.274380 -0.043531 0.115(3) Uiso 0.5 1 d . . P A -1
C1 C 0.3632(3) 0.38454(14) 0.2224(3) 0.0345(7) Uani 1 1 d . . . . .
C2 C 0.3593(3) 0.31499(14) 0.2227(3) 0.0334(7) Uani 1 1 d . . . . .
C3 C 0.3469(4) 0.28205(14) 0.0914(3) 0.0387(7) Uani 1 1 d . . . . .
H3 H 0.338334 0.303908 0.001777 0.046 Uiso 1 1 calc R U . . .
C4 C 0.3719(4) 0.28230(15) 0.3533(3) 0.0412(8) Uani 1 1 d . . . . .
H4 H 0.380469 0.304181 0.442929 0.049 Uiso 1 1 calc R U . . .
C5 C 0.7281(3) 0.50001(12) 0.2148(3) 0.0272(6) Uani 1 1 d . . . . .
C6 C 0.8690(3) 0.49983(12) 0.3626(3) 0.0260(6) Uani 1 1 d . . . . .
C7 C 1.0153(3) 0.46566(12) 0.3807(3) 0.0264(6) Uani 1 1 d . . . . .
H7 H 1.025630 0.442107 0.299072 0.032 Uiso 1 1 calc R U . . .
C8 C 0.8538(3) 0.53420(13) 0.4827(3) 0.0273(6) Uani 1 1 d . . . . .
H8 H 0.753807 0.557479 0.470874 0.033 Uiso 1 1 calc R U . . .
C9 C 0.0801(3) 0.57668(14) 0.1304(3) 0.0350(7) Uani 1 1 d . . . . .
H9 H 0.024651 0.563623 0.029823 0.042 Uiso 1 1 calc R U . . .
C10 C -0.0018(4) 0.61778(14) 0.1943(3) 0.0398(8) Uani 1 1 d . . . . .
H10 H -0.112484 0.631891 0.138758 0.048 Uiso 1 1 calc R U . . .
C11 C 0.0777(4) 0.63853(14) 0.3396(3) 0.0401(7) Uani 1 1 d . . . . .
C12 C 0.2372(4) 0.61470(14) 0.4164(3) 0.0385(7) Uani 1 1 d . . . . .
H12 H 0.295510 0.627492 0.516736 0.046 Uiso 1 1 calc R U . . .
C13 C 0.3107(3) 0.57277(14) 0.3479(3) 0.0332(7) Uani 1 1 d . . . . .
H13 H 0.418543 0.556180 0.403377 0.040 Uiso 1 1 calc R U . . .
C14 C 0.0021(4) 0.68972(15) 0.4044(4) 0.0504(8) Uani 1 1 d . . . . .
H14A H 0.041316 0.687155 0.515464 0.060 Uiso 1 1 calc R U . . .
H14B H -0.123229 0.687442 0.366028 0.060 Uiso 1 1 calc R U . . .
C15 C 0.0639(7) 0.750000 0.3529(6) 0.0585(14) Uani 1 2 d S T P . .
H15A H 0.189381 0.750000 0.390506 0.070 Uiso 1 2 calc R U P . .
H15B H 0.026976 0.750000 0.241731 0.070 Uiso 1 2 calc R U P . .
C16 C 0.556220 0.290030 -0.172339 0.122(4) Uiso 0.5 1 d . . P A -1
H16 H 0.557402 0.333827 -0.182235 0.146 Uiso 0.5 1 calc R U P A -1
C17 C 0.763210 0.312550 0.083710 0.125(4) Uiso 0.5 1 d . . P A -1
H17A H 0.727401 0.355557 0.058377 0.187 Uiso 0.5 1 calc R U P A -1
H17B H 0.887004 0.309967 0.114424 0.187 Uiso 0.5 1 calc R U P A -1
H17C H 0.725774 0.298545 0.166400 0.187 Uiso 0.5 1 calc R U P A -1
C18 C 0.716169 0.209419 -0.031310 0.264(13) Uiso 0.5 1 d . . P A -1
H18A H 0.607148 0.188140 -0.073771 0.397 Uiso 0.5 1 calc R U P A -1
H18B H 0.767588 0.198082 0.074797 0.397 Uiso 0.5 1 calc R U P A -1
H18C H 0.791743 0.197117 -0.086505 0.397 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 O3 113.46(9) . .
O1 Zn1 O4 102.77(8) . 3_665
O3 Zn1 O4 117.85(8) . 3_665
O1 Zn1 N1 124.75(10) . .
O3 Zn1 N1 100.02(8) . .
O4 Zn1 N1 98.16(8) 3_665 .
C1 O1 Zn1 112.40(18) . .
C5 O3 Zn1 127.92(17) . .
C5 O4 Zn1 122.86(16) . 3_665
C9 N1 C13 117.7(2) . .
C9 N1 Zn1 122.32(18) . .
C13 N1 Zn1 119.89(18) . .
C16 N2 C17 126.415(2) . .
C16 N2 C18 111.6 . .
C17 N2 C18 119.673(1) . .
O2 C1 O1 122.8(3) . .
O2 C1 C2 121.6(3) . .
O1 C1 C2 115.6(2) . .
C4 C2 C3 119.1(3) . .
C4 C2 C1 120.8(3) . .
C3 C2 C1 120.1(3) . .
C3 C3 C2 120.48(17) 4_565 .
C3 C3 H3 119.8 4_565 .
C2 C3 H3 119.8 . .
C2 C4 C4 120.41(17) . 4_565
C2 C4 H4 119.8 . .
C4 C4 H4 119.8 4_565 .
O4 C5 O3 124.3(2) . .
O4 C5 C6 118.1(2) . .
O3 C5 C6 117.6(2) . .
C7 C6 C8 119.8(2) . .
C7 C6 C5 120.3(2) . .
C8 C6 C5 119.9(2) . .
C8 C7 C6 120.3(2) 3_766 .
C8 C7 H7 119.9 3_766 .
C6 C7 H7 119.9 . .
C7 C8 C6 119.9(2) 3_766 .
C7 C8 H8 120.0 3_766 .
C6 C8 H8 120.0 . .
N1 C9 C10 122.6(2) . .
N1 C9 H9 118.7 . .
C10 C9 H9 118.7 . .
C9 C10 C11 119.8(3) . .
C9 C10 H10 120.1 . .
C11 C10 H10 120.1 . .
C10 C11 C12 117.3(3) . .
C10 C11 C14 120.8(3) . .
C12 C11 C14 121.5(3) . .
C13 C12 C11 120.2(3) . .
C13 C12 H12 119.9 . .
C11 C12 H12 119.9 . .
N1 C13 C12 122.3(2) . .
N1 C13 H13 118.8 . .
C12 C13 H13 118.8 . .
C11 C14 C15 105.2(3) . .
C11 C14 H14A 110.7 . .
C15 C14 H14A 110.7 . .
C11 C14 H14B 110.7 . .
C15 C14 H14B 110.7 . .
H14A C14 H14B 108.8 . .
C14 C15 C14 115.6(4) 4_575 .
C14 C15 H15A 108.4 4_575 .
C14 C15 H15A 108.4 . .
C14 C15 H15B 108.4 4_575 .
C14 C15 H15B 108.4 . .
H15A C15 H15B 107.4 . .
O5 C16 N2 145.666(1) . .
O5 C16 H16 107.2 . .
N2 C16 H16 107.2 . .
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 1.925(2) .
Zn1 O3 1.9588(17) .
Zn1 O4 1.9885(16) 3_665
Zn1 N1 2.001(2) .
O1 C1 1.291(3) .
O2 C1 1.223(3) .
O3 C5 1.259(3) .
O4 C5 1.258(3) .
O5 C16 1.19635(3) .
N1 C9 1.344(3) .
N1 C13 1.348(3) .
N2 C16 1.39321(4) .
N2 C17 1.41584(3) .
N2 C18 1.41724(5) .
C1 C2 1.501(4) .
C2 C4 1.393(4) .
C2 C3 1.401(4) .
C3 C3 1.383(6) 4_565
C3 H3 0.9500 .
C4 C4 1.394(6) 4_565
C4 H4 0.9500 .
C5 C6 1.497(3) .
C6 C7 1.390(4) .
C6 C8 1.395(4) .
C7 C8 1.386(3) 3_766
C7 H7 0.9500 .
C8 H8 0.9500 .
C9 C10 1.376(4) .
C9 H9 0.9500 .
C10 C11 1.384(4) .
C10 H10 0.9500 .
C11 C12 1.388(4) .
C11 C14 1.500(4) .
C12 C13 1.371(4) .
C12 H12 0.9500 .
C13 H13 0.9500 .
C14 C15 1.537(4) .
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 .
