#------------------------------------------------------------------------------
#$Date: 2019-11-22 23:21:16 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231552 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/33/4003378.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_4003378
loop_
_publ_author_name
'Qi, Yi'
'Xu, Huoshu'
'Li, Xiaomin'
'Tu, Binbin'
'Pang, Qingqing'
'Lin, Xiao'
'Ning, Erlong'
'Li, Qiaowei'
_publ_section_title
;
 Structure Transformation of a Luminescent Pillared-Layer Metal--Organic
 Framework Caused by Point Defects Accumulation
;
_journal_issue                   15
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5478
_journal_paper_doi               10.1021/acs.chemmater.8b02511
_journal_volume                  30
_journal_year                    2018
_chemical_formula_sum            'C28 H18 N O4 Zn'
_chemical_formula_weight         497.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 131.61(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.03(4)
_cell_length_b                   21.02(4)
_cell_length_c                   15.27(3)
_cell_measurement_reflns_used    257
_cell_measurement_temperature    258(2)
_cell_measurement_theta_max      19.54
_cell_measurement_theta_min      2.32
_cell_volume                     5287(18)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      258(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3005
_diffrn_reflns_av_unetI/netI     0.1942
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8490
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        20.290
_diffrn_reflns_theta_max         20.290
_diffrn_reflns_theta_min         1.649
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.579
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2557
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1661
_refine_ls_R_factor_gt           0.1419
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²+80.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3596
_refine_ls_wR_factor_ref         0.3777
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1686
_reflns_number_total             2557
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm8b02511_si_002.cif
_cod_data_source_block           FDM-22
_cod_original_cell_volume        5287(16)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4003378
_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'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Zn1 Zn 0.05892(11) 1.0000 0.62961(16) 0.0364(10) Uani 1 2 d S T P
N1 N 0.1409(11) 1.0000 0.8075(17) 0.069(5) Uani 1 2 d S TU P
O1 O -0.0192(5) 0.9345(5) 0.6007(7) 0.071(3) Uani 1 1 d . . .
O2 O -0.1101(5) 0.9341(5) 0.4012(8) 0.068(3) Uani 1 1 d . . .
C1 C -0.0825(8) 0.9149(6) 0.4999(11) 0.043(3) Uani 1 1 d . U .
C2 C -0.1317(8) 0.8642(6) 0.5007(11) 0.046(3) Uani 1 1 d . . .
C3 C -0.2019(9) 0.8401(8) 0.3961(11) 0.079(5) Uani 1 1 d . . .
H3 H -0.2173 0.8517 0.3250 0.095 Uiso 1 1 calc R U .
C4 C -0.2476(9) 0.7993(8) 0.3996(11) 0.084(6) Uani 1 1 d . . .
H4 H -0.2980 0.7878 0.3289 0.100 Uiso 1 1 calc R U .
C5 C -0.2251(7) 0.7743(7) 0.4980(11) 0.054(4) Uani 1 1 d . . .
C6 C -0.1543(10) 0.7955(8) 0.6014(13) 0.081(5) Uani 1 1 d . U .
H6 H -0.1370 0.7806 0.6723 0.098 Uiso 1 1 calc R U .
C7 C -0.1068(9) 0.8413(8) 0.5992(12) 0.070(4) Uani 1 1 d . U .
H7 H -0.0575 0.8549 0.6694 0.084 Uiso 1 1 calc R U .
C8 C 0.2111(16) 1.0000 0.865(2) 0.119(9) Uani 1 2 d S TU P
H8 H 0.2303 1.0000 0.8260 0.142 Uiso 1 2 calc R U P
C9 C 0.2693(16) 1.0000 0.988(2) 0.125(9) Uani 1 2 d S TU P
H9 H 0.3242 1.0000 1.0263 0.151 Uiso 1 2 calc R U P
C10 C 0.2497(13) 1.0000 1.0469(19) 0.073(6) Uani 1 2 d S TU P
C11 C 0.1689(17) 1.0000 0.987(3) 0.141(11) Uani 1 2 d S TU P
H11 H 0.1496 1.0000 1.0260 0.169 Uiso 1 2 calc R U P
C12 C 0.1174(17) 1.0000 0.868(3) 0.22(3) Uani 1 2 d S T P
H12 H 0.0619 1.0000 0.8258 0.269 Uiso 1 2 calc R U P
C13 C 0.3058(18) 1.0000 1.179(2) 0.111(10) Uani 1 2 d S TU P
H13 H 0.2827 1.0000 1.2129 0.134 Uiso 1 2 calc R U P
C14 C 0.3829(19) 1.0000 1.247(2) 0.111(10) Uani 1 2 d S TU P
H14 H 0.4039 1.0000 1.2108 0.133 Uiso 1 2 calc R U P
C15 C 0.4418(14) 1.0000 1.3740(19) 0.090(8) Uani 1 2 d S T P
C16 C 0.4338(18) 1.0458(17) 1.438(2) 0.071(9) Uani 0.5 1 d . U P
C17 C 0.3649(19) 1.0852(19) 1.381(3) 0.100(13) Uani 0.5 1 d . . P
H17 H 0.3235 1.0820 1.3004 0.119 Uiso 0.5 1 calc R U P
C18 C 0.356(3) 1.130(3) 1.443(4) 0.19(3) Uani 0.5 1 d . . P
H18 H 0.3156 1.1614 1.4062 0.230 Uiso 0.5 1 calc R U P
C19 C 0.5087(19) 0.9609(16) 1.431(3) 0.077(9) Uani 0.5 1 d . U P
C20 C 0.516(3) 0.921(2) 1.370(4) 0.107(14) Uani 0.5 1 d . . P
H20 H 0.4762 0.9207 1.2889 0.129 Uiso 0.5 1 calc R U P
C21 C 0.581(3) 0.879(3) 1.426(4) 0.139(19) Uani 0.5 1 d . . P
H21 H 0.5856 0.8553 1.3793 0.167 Uiso 0.5 1 calc R U P
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 O1 86.4(6) . 6_575
O1 Zn1 O2 160.6(4) . 5_576
O1 Zn1 O2 90.5(5) 6_575 5_576
O1 Zn1 O2 90.5(5) . 2_556
O1 Zn1 O2 160.6(4) 6_575 2_556
O2 Zn1 O2 86.2(6) 5_576 2_556
O1 Zn1 N1 99.5(5) . .
O1 Zn1 N1 99.5(5) 6_575 .
O2 Zn1 N1 99.9(5) 5_576 .
O2 Zn1 N1 99.9(5) 2_556 .
O1 Zn1 Zn1 81.0(3) . 5_576
O1 Zn1 Zn1 81.0(3) 6_575 5_576
O2 Zn1 Zn1 79.6(3) 5_576 5_576
O2 Zn1 Zn1 79.6(3) 2_556 5_576
N1 Zn1 Zn1 179.3(5) . 5_576
C8 N1 C12 114(2) . .
C8 N1 Zn1 124.3(18) . .
C12 N1 Zn1 121.3(17) . .
C1 O1 Zn1 125.1(8) . .
C1 O2 Zn1 126.5(8) . 5_576
O2 C1 O1 127.7(12) . .
O2 C1 C2 116.9(11) . .
O1 C1 C2 115.4(11) . .
C7 C2 C3 119.1(12) . .
C7 C2 C1 120.7(12) . .
C3 C2 C1 120.2(11) . .
C4 C3 C2 118.6(12) . .
C4 C3 H3 120.7 . .
C2 C3 H3 120.7 . .
C5 C4 C3 124.3(12) . .
C5 C4 H4 117.8 . .
C3 C4 H4 117.8 . .
C4 C5 C6 117.3(12) . .
C4 C5 C5 124.5(14) . 7_466
C6 C5 C5 118.2(14) . 7_466
C5 C6 C7 118.8(13) . .
C5 C6 H6 120.6 . .
C7 C6 H6 120.6 . .
C2 C7 C6 121.3(13) . .
C2 C7 H7 119.4 . .
C6 C7 H7 119.4 . .
N1 C8 C9 125(2) . .
N1 C8 H8 117.3 . .
C9 C8 H8 117.3 . .
C10 C9 C8 122(3) . .
C10 C9 H9 119.1 . .
C8 C9 H9 119.1 . .
C9 C10 C11 117(3) . .
C9 C10 C13 127(2) . .
C11 C10 C13 116(2) . .
C10 C11 C12 117(3) . .
C10 C11 H11 121.6 . .
C12 C11 H11 121.6 . .
N1 C12 C11 125(3) . .
N1 C12 H12 117.7 . .
C11 C12 H12 117.7 . .
C14 C13 C10 123(2) . .
C14 C13 H13 118.4 . .
C10 C13 H13 118.4 . .
C13 C14 C15 128(3) . .
C13 C14 H14 116.1 . .
C15 C14 H14 116.1 . .
C19 C15 C19 73(3) 6_575 .
C19 C15 C14 119(2) 6_575 .
C19 C15 C14 119(2) . .
C19 C15 C16 74.7(19) 6_575 .
C19 C15 C16 121(2) . .
C14 C15 C16 119.7(19) . .
C19 C15 C16 121(2) 6_575 6_575
C19 C15 C16 74.7(19) . 6_575
C14 C15 C16 119.7(19) . 6_575
C16 C15 C16 82(3) . 6_575
C17 C16 C15 122(2) . .
C17 C16 C19 119(3) . 5_678
C15 C16 C19 117(3) . 5_678
C17 C16 C19 134(3) . 6_575
C15 C16 C19 50.4(16) . 6_575
C19 C16 C19 94(2) 5_678 6_575
C17 C16 C16 126(2) . 6_575
C15 C16 C16 48.9(14) . 6_575
C19 C16 C16 84.6(19) 5_678 6_575
C19 C16 C16 85.3(16) 6_575 6_575
C16 C17 C18 123(3) . .
C16 C17 H17 118.5 . .
C18 C17 H17 118.5 . .
C17 C18 C21 112(4) . 5_678
C17 C18 H18 124.0 . .
C21 C18 H18 124.1 5_678 .
C20 C19 C15 120(3) . .
C20 C19 C16 119(3) . 5_678
C15 C19 C16 120(3) . 5_678
C20 C19 C19 129(2) . 6_575
C15 C19 C19 53.4(15) . 6_575
C16 C19 C19 95.4(19) 5_678 6_575
C20 C19 C16 123(3) . 6_575
C15 C19 C16 54.9(16) . 6_575
C16 C19 C16 85(2) 5_678 6_575
C19 C19 C16 94.7(16) 6_575 6_575
C19 C20 C21 122(4) . .
C19 C20 H20 119.2 . .
C21 C20 H20 119.2 . .
C20 C21 C18 124(4) . 5_678
C20 C21 H21 117.9 . .
C18 C21 H21 117.9 5_678 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 2.012(11) .
Zn1 O1 2.012(11) 6_575
Zn1 O2 2.029(10) 5_576
Zn1 O2 2.029(10) 2_556
Zn1 N1 2.03(2) .
Zn1 Zn1 2.959(6) 5_576
N1 C8 1.17(3) .
N1 C12 1.32(4) .
O1 C1 1.278(14) .
O2 C1 1.260(14) .
O2 Zn1 2.029(10) 5_576
C1 C2 1.525(17) .
C2 C7 1.304(17) .
C2 C3 1.386(17) .
C3 C4 1.349(19) .
C3 H3 0.9300 .
C4 C5 1.339(17) .
C4 H4 0.9300 .
C5 C6 1.361(18) .
C5 C5 1.53(2) 7_466
C6 C7 1.44(2) .
C6 H6 0.9300 .
C7 H7 0.9300 .
C8 C9 1.41(4) .
C8 H8 0.9300 .
C9 C10 1.22(3) .
C9 H9 0.9300 .
C10 C11 1.36(3) .
C10 C13 1.52(3) .
C11 C12 1.37(4) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C13 C14 1.27(3) .
C13 H13 0.9300 .
C14 C15 1.45(3) .
C14 H14 0.9300 .
C15 C19 1.38(3) 6_575
C15 C19 1.38(3) .
C15 C16 1.46(3) .
C15 C16 1.46(3) 6_575
C16 C17 1.41(5) .
C16 C19 1.50(4) 5_678
C16 C19 1.73(4) 6_575
C16 C16 1.93(7) 6_575
C17 C18 1.44(5) .
C17 H17 0.9300 .
C18 C21 1.52(6) 5_678
C18 H18 0.9300 .
C19 C20 1.34(5) .
C19 C16 1.50(4) 5_678
C19 C19 1.65(7) 6_575
C19 C16 1.73(4) 6_575
C20 C21 1.39(6) .
C20 H20 0.9300 .
C21 C18 1.52(6) 5_678
C21 H21 0.9300 .
