#------------------------------------------------------------------------------
#$Date: 2016-03-05 09:47:16 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177661 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/85/7118548.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_7118548
loop_
_publ_author_name
'Lama, Prem'
'Alimi, Lukman O.'
'Das, Raj Kumar'
'Barbour, Leonard J.'
_publ_section_title
;
 Hydration-dependent anomalous thermal expansion behaviour in a
 coordination polymer.
;
_journal_issue                   15
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3231
_journal_page_last               3234
_journal_paper_doi               10.1039/c6cc00158k
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C22 H18 N2 O6 Zn'
_chemical_formula_sum            'C22 H18 N2 O6 Zn'
_chemical_formula_weight         471.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-12-09 deposited with the CCDC.
2016-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.976(2)
_cell_length_b                   7.7768(8)
_cell_length_c                   13.6920(14)
_cell_measurement_reflns_used    3215
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      25.81
_cell_measurement_theta_min      2.61
_cell_volume                     2020.6(4)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'X-Seed (Barbour 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10418
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    1.259
_exptl_absorpt_correction_T_max  0.7996
_exptl_absorpt_correction_T_min  0.5449
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.549
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.186
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3908
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0408P)²+0.5885P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0893
_reflns_number_gt                3475
_reflns_number_total             3908
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc00158k2.cif
_cod_data_source_block           LJB_1_160K
_cod_depositor_comments
'Adding full bibliography for 7118534--7118552.cif.'
_cod_original_sg_symbol_Hall     P2c-2n
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               7118548
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'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
Zn1 Zn 0.391105(17) 1.05973(5) 0.79469(3) 0.01258(11) Uani 1 1 d .
O1 O 0.47142(14) 0.9432(3) 0.85439(18) 0.0187(6) Uani 1 1 d .
O2 O 0.49904(15) 0.7732(4) 0.7285(2) 0.0305(7) Uani 1 1 d .
O3 O 0.76516(15) 0.6686(4) 0.7173(2) 0.0337(8) Uani 1 1 d .
O4 O 0.80915(14) 0.5514(3) 0.85297(18) 0.0198(6) Uani 1 1 d .
O5 O 0.69739(15) 0.7305(4) 1.17022(19) 0.0292(7) Uani 1 1 d .
O6 O 0.59713(13) 0.8786(4) 1.15945(18) 0.0199(6) Uani 1 1 d .
N1 N 0.39770(15) 1.2720(4) 0.8840(2) 0.0166(7) Uani 1 1 d .
N2 N 0.32559(18) 1.7867(4) 1.5456(2) 0.0245(8) Uani 1 1 d .
H2 H 0.3142 1.7856 1.6079 0.029 Uiso 1 1 calc R
C1 C 0.51152(18) 0.8361(5) 0.8090(3) 0.0167(8) Uani 1 1 d .
C2 C 0.57811(18) 0.7898(5) 0.8627(3) 0.0143(8) Uani 1 1 d .
C3 C 0.63685(18) 0.7329(4) 0.8125(2) 0.0149(8) Uani 1 1 d .
H3 H 0.6354 0.7252 0.7433 0.018 Uiso 1 1 calc R
C4 C 0.69829(18) 0.6867(5) 0.8619(3) 0.0153(8) Uani 1 1 d .
C5 C 0.76199(17) 0.6320(4) 0.8048(3) 0.0169(8) Uani 1 1 d .
C6 C 0.70029(19) 0.6980(5) 0.9634(2) 0.0158(8) Uani 1 1 d .
H6 H 0.7411 0.6612 0.9978 0.019 Uiso 1 1 calc R
C7 C 0.64321(19) 0.7625(5) 1.0144(2) 0.0146(8) Uani 1 1 d .
C8 C 0.64796(19) 0.7888(5) 1.1235(3) 0.0179(8) Uani 1 1 d .
C9 C 0.58245(19) 0.8083(5) 0.9638(2) 0.0151(8) Uani 1 1 d .
H9 H 0.5433 0.8530 0.9988 0.018 Uiso 1 1 calc R
C10 C 0.38641(19) 1.4347(5) 0.8544(3) 0.0180(8) Uani 1 1 d .
H10 H 0.3758 1.4551 0.7876 0.022 Uiso 1 1 calc R
C11 C 0.3897(2) 1.5736(5) 0.9176(3) 0.0208(9) Uani 1 1 d .
H11 H 0.3806 1.6863 0.8941 0.025 Uiso 1 1 calc R
C12 C 0.4063(2) 1.5482(5) 1.0151(3) 0.0189(8) Uani 1 1 d .
C13 C 0.4201(2) 1.3800(5) 1.0451(3) 0.0200(8) Uani 1 1 d .
H13 H 0.4333 1.3569 1.1107 0.024 Uiso 1 1 calc R
C14 C 0.4145(2) 1.2478(5) 0.9786(3) 0.0179(8) Uani 1 1 d .
H14 H 0.4229 1.1337 1.0006 0.021 Uiso 1 1 calc R
C15 C 0.4098(2) 1.6981(6) 1.0854(3) 0.0266(10) Uani 1 1 d .
H15A H 0.3831 1.7955 1.0570 0.032 Uiso 1 1 calc R
H15B H 0.4595 1.7347 1.0915 0.032 Uiso 1 1 calc R
C16 C 0.3808(2) 1.6613(6) 1.1878(3) 0.0233(9) Uani 1 1 d .
H16A H 0.3321 1.6165 1.1828 0.028 Uiso 1 1 calc R
H16B H 0.4101 1.5729 1.2202 0.028 Uiso 1 1 calc R
C17 C 0.3812(3) 1.8238(6) 1.2473(3) 0.0296(12) Uani 1 1 d .
H17A H 0.3481 1.9070 1.2173 0.036 Uiso 1 1 calc R
H17B H 0.4289 1.8747 1.2447 0.036 Uiso 1 1 calc R
C18 C 0.3609(2) 1.7982(6) 1.3527(3) 0.0253(10) Uani 1 1 d .
C19 C 0.2927(2) 1.8290(7) 1.3822(3) 0.0379(12) Uani 1 1 d .
H19 H 0.2571 1.8530 1.3354 0.045 Uiso 1 1 calc R
C20 C 0.2766(2) 1.8246(7) 1.4805(3) 0.0370(12) Uani 1 1 d .
H20 H 0.2299 1.8490 1.5015 0.044 Uiso 1 1 calc R
C21 C 0.3916(2) 1.7502(7) 1.5202(3) 0.0309(12) Uani 1 1 d .
H21 H 0.4257 1.7226 1.5685 0.037 Uiso 1 1 calc R
C22 C 0.4095(2) 1.7529(7) 1.4233(3) 0.0333(11) Uani 1 1 d .
H22 H 0.4561 1.7231 1.4043 0.040 Uiso 1 1 calc R
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
O6 Zn1 O4 126.60(11) 2_674 4_465
O6 Zn1 O1 115.31(11) 2_674 .
O4 Zn1 O1 104.22(11) 4_465 .
O6 Zn1 N1 111.40(12) 2_674 .
O4 Zn1 N1 99.25(11) 4_465 .
O1 Zn1 N1 94.35(11) . .
C1 O1 Zn1 124.0(2) . .
C5 O4 Zn1 124.5(3) . 4_565
C8 O6 Zn1 114.5(2) . 2_675
C10 N1 C14 117.3(3) . .
C10 N1 Zn1 124.4(3) . .
C14 N1 Zn1 118.3(3) . .
C20 N2 C21 122.3(4) . .
O2 C1 O1 125.2(3) . .
O2 C1 C2 120.3(3) . .
O1 C1 C2 114.5(3) . .
C3 C2 C9 118.6(3) . .
C3 C2 C1 120.7(3) . .
C9 C2 C1 120.6(3) . .
C2 C3 C4 121.1(3) . .
C6 C4 C3 119.3(3) . .
C6 C4 C5 121.0(3) . .
C3 C4 C5 119.6(3) . .
O3 C5 O4 125.5(3) . .
O3 C5 C4 118.7(3) . .
O4 C5 C4 115.8(4) . .
C7 C6 C4 120.4(3) . .
C6 C7 C9 119.4(3) . .
C6 C7 C8 120.1(3) . .
C9 C7 C8 120.5(3) . .
O5 C8 O6 125.2(4) . .
O5 C8 C7 120.9(3) . .
O6 C8 C7 114.0(3) . .
C7 C9 C2 121.1(3) . .
N1 C10 C11 122.5(3) . .
C12 C11 C10 120.1(4) . .
C11 C12 C13 117.3(4) . .
C11 C12 C15 120.8(4) . .
C13 C12 C15 121.8(3) . .
C14 C13 C12 119.4(3) . .
N1 C14 C13 123.3(4) . .
C12 C15 C16 114.9(3) . .
C17 C16 C15 109.7(4) . .
C16 C17 C18 114.0(4) . .
C19 C18 C22 117.8(4) . .
C19 C18 C17 119.9(4) . .
C22 C18 C17 122.2(4) . .
C18 C19 C20 119.4(4) . .
N2 C20 C19 120.4(4) . .
N2 C21 C22 118.9(4) . .
C21 C22 C18 121.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O6 1.926(3) 2_674
Zn1 O4 1.950(3) 4_465
Zn1 O1 1.952(3) .
Zn1 N1 2.058(3) .
O1 C1 1.288(4) .
O2 C1 1.229(5) .
O3 C5 1.234(5) .
O4 C5 1.276(4) .
O4 Zn1 1.950(3) 4_565
O5 C8 1.222(4) .
O6 C8 1.289(4) .
O6 Zn1 1.926(3) 2_675
N1 C10 1.346(5) .
N1 C14 1.347(5) .
N2 C20 1.321(5) .
N2 C21 1.330(6) .
C1 C2 1.505(5) .
C2 C3 1.382(5) .
C2 C9 1.394(5) .
C3 C4 1.395(5) .
C4 C6 1.394(5) .
C4 C5 1.500(5) .
C6 C7 1.383(5) .
C7 C9 1.392(5) .
C7 C8 1.511(5) .
C10 C11 1.385(5) .
C11 C12 1.385(6) .
C12 C13 1.396(6) .
C12 C15 1.513(6) .
C13 C14 1.378(5) .
C15 C16 1.533(5) .
C16 C17 1.503(6) .
C17 C18 1.507(5) .
C18 C19 1.376(6) .
C18 C22 1.382(6) .
C19 C20 1.381(6) .
C21 C22 1.371(6) .
