#------------------------------------------------------------------------------
#$Date: 2016-03-05 09:47:16 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177661 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/85/7118543.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_7118543
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, H2 O'
_chemical_formula_sum            'C22 H20 N2 O7 Zn'
_chemical_formula_weight         489.77
_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                   19.1136(9)
_cell_length_b                   7.8642(4)
_cell_length_c                   13.7696(6)
_cell_measurement_reflns_used    4878
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.59
_cell_volume                     2069.75(17)
_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      240(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10748
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    1.235
_exptl_absorpt_correction_T_max  0.7956
_exptl_absorpt_correction_T_min  0.6070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4041
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0298P)²+0.3787P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                3783
_reflns_number_total             4041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc00158k2.cif
_cod_data_source_block           LJB_1_H2O_240K
_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               7118543
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 0.386740(12) -0.04567(3) 0.18817(3) 0.01591(9) Uani 1 1 d .
O1 O 0.46748(10) 0.0609(2) 0.12604(14) 0.0220(4) Uani 1 1 d .
O2 O 0.49928(11) 0.2228(3) 0.25088(16) 0.0396(6) Uani 1 1 d .
O3 O 0.76408(12) 0.3055(3) 0.26602(17) 0.0436(6) Uani 1 1 d .
O4 O 0.80688(10) 0.4251(3) 0.13390(16) 0.0292(5) Uani 1 1 d .
O5 O 0.69910(11) 0.2487(3) -0.18492(16) 0.0377(6) Uani 1 1 d .
O6 O 0.59993(10) 0.1028(3) -0.17711(15) 0.0266(5) Uani 1 1 d .
N1 N 0.38815(11) -0.2554(3) 0.09805(18) 0.0209(5) Uani 1 1 d .
N2 N 0.33173(14) -0.7718(4) -0.5619(2) 0.0383(7) Uani 1 1 d .
H2 H 0.3170 -0.7762 -0.6216 0.046 Uiso 1 1 calc R
C1 C 0.50988(12) 0.1593(4) 0.17118(19) 0.0200(6) Uani 1 1 d .
C2 C 0.57720(13) 0.1969(3) 0.1173(2) 0.0171(5) Uani 1 1 d .
C3 C 0.63579(12) 0.2486(3) 0.16941(18) 0.0171(6) Uani 1 1 d .
H3 H 0.6334 0.2563 0.2374 0.021 Uiso 1 1 calc R
C4 C 0.69802(13) 0.2891(4) 0.1220(2) 0.0197(6) Uani 1 1 d .
C5 C 0.76067(12) 0.3443(3) 0.1797(2) 0.0213(6) Uani 1 1 d .
C6 C 0.70119(13) 0.2765(4) 0.02115(19) 0.0202(6) Uani 1 1 d .
H6 H 0.7422 0.3084 -0.0118 0.024 Uiso 1 1 calc R
C7 C 0.64379(14) 0.2168(3) -0.0311(2) 0.0195(6) Uani 1 1 d .
C8 C 0.64924(14) 0.1909(4) -0.13880(19) 0.0215(6) Uani 1 1 d .
C9 C 0.58184(13) 0.1761(3) 0.01795(19) 0.0182(6) Uani 1 1 d .
H9 H 0.5432 0.1345 -0.0170 0.022 Uiso 1 1 calc R
C10 C 0.38248(15) -0.4181(4) 0.1261(2) 0.0262(7) Uani 1 1 d .
H10 H 0.3730 -0.4417 0.1917 0.031 Uiso 1 1 calc R
C11 C 0.39008(15) -0.5521(4) 0.0622(2) 0.0287(7) Uani 1 1 d .
H11 H 0.3845 -0.6644 0.0843 0.034 Uiso 1 1 calc R
C12 C 0.40591(16) -0.5214(4) -0.0346(2) 0.0260(6) Uani 1 1 d .
C13 C 0.41176(16) -0.3527(4) -0.0628(2) 0.0291(7) Uani 1 1 d .
H13 H 0.4223 -0.3252 -0.1276 0.035 Uiso 1 1 calc R
C14 C 0.40212(16) -0.2266(4) 0.0044(2) 0.0258(6) Uani 1 1 d .
H14 H 0.4055 -0.1131 -0.0165 0.031 Uiso 1 1 calc R
C15 C 0.4171(2) -0.6642(4) -0.1054(2) 0.0366(8) Uani 1 1 d .
H15A H 0.3951 -0.7668 -0.0789 0.044 Uiso 1 1 calc R
H15B H 0.4675 -0.6863 -0.1098 0.044 Uiso 1 1 calc R
C16 C 0.38925(16) -0.6361(5) -0.2074(2) 0.0355(8) Uani 1 1 d .
H16A H 0.3384 -0.6204 -0.2047 0.043 Uiso 1 1 calc R
H16B H 0.4099 -0.5322 -0.2344 0.043 Uiso 1 1 calc R
C17 C 0.4060(2) -0.7841(5) -0.2730(3) 0.0486(11) Uani 1 1 d .
H17A H 0.4570 -0.7969 -0.2762 0.058 Uiso 1 1 calc R
H17B H 0.3870 -0.8878 -0.2437 0.058 Uiso 1 1 calc R
C18 C 0.37827(17) -0.7696(4) -0.3749(3) 0.0343(8) Uani 1 1 d .
C19 C 0.30818(18) -0.7942(6) -0.3952(3) 0.0489(10) Uani 1 1 d .
H19 H 0.2759 -0.8100 -0.3445 0.059 Uiso 1 1 calc R
C20 C 0.28595(19) -0.7954(6) -0.4907(3) 0.0529(11) Uani 1 1 d .
H20 H 0.2384 -0.8130 -0.5053 0.063 Uiso 1 1 calc R
C21 C 0.39799(19) -0.7423(6) -0.5458(3) 0.0462(10) Uani 1 1 d .
H21 H 0.4289 -0.7247 -0.5980 0.055 Uiso 1 1 calc R
C22 C 0.42232(18) -0.7372(5) -0.4508(3) 0.0449(9) Uani 1 1 d .
H22 H 0.4695 -0.7112 -0.4386 0.054 Uiso 1 1 calc R
O1W O 0.70399(19) 0.0121(5) 0.3540(3) 0.0865(11) Uani 1 1 d D
H2W1 H 0.7382 -0.0621 0.3479 0.050 Uiso 1 1 d D
H1W1 H 0.7269 0.1139 0.3521 0.050 Uiso 1 1 d D
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 125.96(9) 2_655 4_455
O6 Zn1 O1 114.67(8) 2_655 .
O4 Zn1 O1 104.03(9) 4_455 .
O6 Zn1 N1 113.02(10) 2_655 .
O4 Zn1 N1 99.72(9) 4_455 .
O1 Zn1 N1 93.96(8) . .
C1 O1 Zn1 123.12(18) . .
C5 O4 Zn1 127.2(2) . 4
C8 O6 Zn1 115.14(18) . 2_654
C14 N1 C10 117.1(3) . .
C14 N1 Zn1 116.6(2) . .
C10 N1 Zn1 126.0(2) . .
C21 N2 C20 122.7(3) . .
O2 C1 O1 125.3(2) . .
O2 C1 C2 120.0(2) . .
O1 C1 C2 114.7(2) . .
C9 C2 C3 119.6(2) . .
C9 C2 C1 121.1(2) . .
C3 C2 C1 119.3(2) . .
C2 C3 C4 120.8(2) . .
C3 C4 C6 119.2(2) . .
C3 C4 C5 120.0(2) . .
C6 C4 C5 120.9(2) . .
O3 C5 O4 125.0(2) . .
O3 C5 C4 118.8(2) . .
O4 C5 C4 116.2(3) . .
C7 C6 C4 120.3(2) . .
C6 C7 C9 119.6(3) . .
C6 C7 C8 120.1(2) . .
C9 C7 C8 120.3(2) . .
O5 C8 O6 123.7(3) . .
O5 C8 C7 120.9(2) . .
O6 C8 C7 115.4(2) . .
C2 C9 C7 120.3(2) . .
N1 C10 C11 122.4(3) . .
C10 C11 C12 120.1(3) . .
C13 C12 C11 117.0(3) . .
C13 C12 C15 121.4(3) . .
C11 C12 C15 121.6(3) . .
C14 C13 C12 119.5(3) . .
N1 C14 C13 123.8(3) . .
C12 C15 C16 116.2(3) . .
C17 C16 C15 111.6(3) . .
C18 C17 C16 115.2(3) . .
C22 C18 C19 118.0(3) . .
C22 C18 C17 120.7(3) . .
C19 C18 C17 121.3(4) . .
C18 C19 C20 119.4(3) . .
N2 C20 C19 119.9(3) . .
N2 C21 C22 119.3(3) . .
C18 C22 C21 120.6(3) . .
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(2) 2_655
Zn1 O4 1.946(2) 4_455
Zn1 O1 1.9532(19) .
Zn1 N1 2.064(2) .
O1 C1 1.282(3) .
O2 C1 1.223(4) .
O3 C5 1.229(4) .
O4 C5 1.257(3) .
O4 Zn1 1.946(2) 4
O5 C8 1.232(3) .
O6 C8 1.283(3) .
O6 Zn1 1.926(2) 2_654
N1 C14 1.336(4) .
N1 C10 1.341(4) .
N2 C21 1.306(5) .
N2 C20 1.326(5) .
C1 C2 1.514(3) .
C2 C9 1.381(4) .
C2 C3 1.391(4) .
C3 C4 1.394(4) .
C4 C6 1.394(4) .
C4 C5 1.501(4) .
C6 C7 1.393(4) .
C7 C9 1.400(4) .
C7 C8 1.501(4) .
C10 C11 1.381(4) .
C11 C12 1.387(5) .
C12 C13 1.386(4) .
C12 C15 1.503(4) .
C13 C14 1.369(4) .
C15 C16 1.518(4) .
C16 C17 1.508(5) .
C17 C18 1.504(5) .
C18 C22 1.366(5) .
C18 C19 1.382(5) .
C19 C20 1.383(5) .
C21 C22 1.389(5) .
