#------------------------------------------------------------------------------
#$Date: 2015-12-06 07:55:39 +0200 (Sun, 06 Dec 2015) $
#$Revision: 170778 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/36/4513617.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_4513617
loop_
_publ_author_name
'Husain, Ahmad'
'Parveen, Rumana'
'Dastidar, Parthasarathi'
_publ_section_title
;
 New Series of ZnII/CdIIMixed Ligand Coordination Polymers: Toward the
 Design of Metallogels
;
_journal_issue                   10
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5075
_journal_paper_doi               10.1021/acs.cgd.5b01044
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C24 H18 N4 O6 Zn, H2 O'
_chemical_formula_sum            'C24 H20 N4 O7 Zn'
_chemical_formula_weight         541.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                112.112(7)
_cell_angle_beta                 110.466(7)
_cell_angle_gamma                100.432(8)
_cell_formula_units_Z            2
_cell_length_a                   9.540(7)
_cell_length_b                   12.277(9)
_cell_length_c                   12.440(9)
_cell_measurement_reflns_used    9769
_cell_measurement_temperature    275(2)
_cell_measurement_theta_max      26.51
_cell_measurement_theta_min      2.34
_cell_volume                     1179.7(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      275(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31822
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.403
_diffrn_reflns_theta_min         1.919
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.532
_exptl_crystal_size_mid          0.375
_exptl_crystal_size_min          0.170
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.6375
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         4838
_refine_ls_number_restraints     303
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0395P)²+0.5076P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4469
_reflns_number_total             4838
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b01044_si_006.cif
_cod_data_source_block           CP5
_cod_depositor_comments
'Adding full bibliography for 4513613--4513620.cif.'
_cod_original_cell_volume        1179.8(14)
_cod_database_code               4513617
_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.
;
_shelx_estimated_absorpt_t_min   0.594
_shelx_estimated_absorpt_t_max   0.836
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
C1 C 0.2589(3) -0.0289(2) -0.11096(19) 0.0516(6) Uani 1 1 d . U
C2 C 0.3899(4) 0.0838(2) -0.0314(2) 0.0702(8) Uani 1 1 d . U
H2 H 0.4546 0.1098 -0.0649 0.084 Uiso 1 1 calc R U
C3 C 0.4251(3) 0.1577(2) 0.0966(2) 0.0563(6) Uani 1 1 d . U
H3 H 0.5125 0.2332 0.1489 0.068 Uiso 1 1 calc R U
C4 C 0.3290(2) 0.11858(18) 0.14754(17) 0.0366(4) Uani 1 1 d . U
C5 C 0.1984(3) 0.0059(2) 0.0679(2) 0.0531(6) Uani 1 1 d . U
H5 H 0.1334 -0.0200 0.1012 0.064 Uiso 1 1 calc R U
C6 C 0.1635(3) -0.0690(2) -0.0615(2) 0.0549(6) Uani 1 1 d . U
H6 H 0.0769 -0.1450 -0.1139 0.066 Uiso 1 1 calc R U
C7 C 0.5227(2) 0.35137(15) 0.48259(15) 0.0259(3) Uani 1 1 d . U
C8 C 0.68418(19) 0.41685(16) 0.57300(16) 0.0267(3) Uani 1 1 d . U
H8 H 0.7628 0.4113 0.5455 0.032 Uiso 1 1 calc R U
C9 C 0.72795(18) 0.49085(15) 0.70510(15) 0.0248(3) Uani 1 1 d . U
C10 C 0.60915(19) 0.50432(15) 0.74425(15) 0.0256(3) Uani 1 1 d . U
H10 H 0.6378 0.5555 0.8315 0.031 Uiso 1 1 calc R U
C11 C 0.44706(18) 0.44134(15) 0.65298(15) 0.0243(3) Uani 1 1 d . U
C12 C 0.40365(19) 0.36349(15) 0.52207(15) 0.0259(3) Uani 1 1 d . U
H12 H 0.2960 0.3199 0.4615 0.031 Uiso 1 1 calc R U
C13 C 0.31940(19) 0.45411(16) 0.69650(15) 0.0268(3) Uani 1 1 d . U
C14 C 0.90200(19) 0.54814(16) 0.80535(16) 0.0279(3) Uani 1 1 d . U
C15 C 0.5051(2) 0.68392(16) 1.11530(17) 0.0328(4) Uani 1 1 d . U
H15 H 0.5332 0.6225 1.0652 0.039 Uiso 1 1 calc R U
C16 C 0.6212(2) 0.77526(16) 1.23868(17) 0.0334(4) Uani 1 1 d . U
H16 H 0.7241 0.7734 1.2710 0.040 Uiso 1 1 calc R U
C17 C 0.5836(2) 0.86991(15) 1.31433(16) 0.0292(3) Uani 1 1 d . U
C18 C 0.4273(2) 0.8659(2) 1.26146(19) 0.0459(5) Uani 1 1 d . U
H18 H 0.3973 0.9279 1.3086 0.055 Uiso 1 1 calc R U
C19 C 0.3157(2) 0.76928(19) 1.13816(18) 0.0427(5) Uani 1 1 d . U
H19 H 0.2105 0.7665 1.1054 0.051 Uiso 1 1 calc R U
C20 C 0.9381(3) 1.04581(18) 1.65010(19) 0.0458(5) Uani 1 1 d . U
H20 H 1.0094 1.0271 1.7074 0.055 Uiso 1 1 calc R U
C21 C 0.8198(3) 0.94717(17) 1.53121(19) 0.0443(5) Uani 1 1 d . U
H21 H 0.8138 0.8646 1.5091 0.053 Uiso 1 1 calc R U
C22 C 0.7100(2) 0.97286(16) 1.44525(16) 0.0302(4) Uani 1 1 d . U
C23 C 0.7269(2) 1.09793(18) 1.48220(19) 0.0434(5) Uani 1 1 d . U
H23 H 0.6558 1.1194 1.4279 0.052 Uiso 1 1 calc R U
C24 C 0.8524(3) 1.19058(18) 1.6021(2) 0.0475(5) Uani 1 1 d . U
H24 H 0.8653 1.2744 1.6246 0.057 Uiso 1 1 calc R U
N1 N 0.35833(19) 0.18846(15) 0.27961(15) 0.0375(3) Uani 1 1 d . U
N2 N 0.49175(18) 0.27697(14) 0.35060(14) 0.0316(3) Uani 1 1 d . U
N3 N 0.35346(16) 0.67961(13) 1.06422(13) 0.0272(3) Uani 1 1 d . U
N4 N 0.95491(19) 1.16662(14) 1.68656(15) 0.0388(4) Uani 1 1 d . U
O1 O 0.2347(3) -0.09385(17) -0.23585(15) 0.0786(6) Uani 1 1 d . U
H1 H 0.1554 -0.1585 -0.2757 0.094 Uiso 1 1 calc R U
O2 O 1.00374(14) 0.53529(13) 0.76018(12) 0.0357(3) Uani 1 1 d . U
O3 O 0.94268(15) 0.59938(15) 0.92357(12) 0.0472(4) Uani 1 1 d . U
O4 O 0.17700(15) 0.38470(14) 0.62046(13) 0.0444(3) Uani 1 1 d . U
O5 O 0.36830(14) 0.53370(12) 0.81607(11) 0.0323(3) Uani 1 1 d . U
O6 O 0.16475(15) 0.38781(11) 0.90319(11) 0.0329(3) Uani 1 1 d . U
H6A H 0.0932 0.3218 0.8307 0.049 Uiso 1 1 d R U
H6B H 0.1298 0.3999 0.9609 0.049 Uiso 1 1 d R U
O7 O 0.0453(3) -0.3315(2) -0.37968(19) 0.1026(9) Uani 1 1 d D .
H7A H 0.024(4) -0.387(3) -0.356(3) 0.123 Uiso 1 1 d D U
H7B H -0.027(3) -0.361(3) -0.4577(17) 0.123 Uiso 1 1 d D U
Zn1 Zn 0.20588(2) 0.53931(2) 0.87684(2) 0.02544(7) Uani 1 1 d . U
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 C1 C6 124.1(2) . .
O1 C1 C2 115.9(2) . .
C6 C1 C2 120.0(2) . .
C3 C2 C1 120.8(2) . .
C3 C2 H2 119.6 . .
C1 C2 H2 119.6 . .
C2 C3 C4 119.7(2) . .
C2 C3 H3 120.1 . .
C4 C3 H3 120.1 . .
C5 C4 C3 119.35(18) . .
C5 C4 N1 117.34(18) . .
C3 C4 N1 123.31(18) . .
C4 C5 C6 120.8(2) . .
C4 C5 H5 119.6 . .
C6 C5 H5 119.6 . .
C1 C6 C5 119.3(2) . .
C1 C6 H6 120.4 . .
C5 C6 H6 120.4 . .
C8 C7 C12 120.34(15) . .
C8 C7 N2 115.33(15) . .
C12 C7 N2 124.30(15) . .
C7 C8 C9 120.03(15) . .
C7 C8 H8 120.0 . .
C9 C8 H8 120.0 . .
C10 C9 C8 119.56(15) . .
C10 C9 C14 120.23(15) . .
C8 C9 C14 120.07(14) . .
C9 C10 C11 120.36(16) . .
C9 C10 H10 119.8 . .
C11 C10 H10 119.8 . .
C12 C11 C10 119.96(15) . .
C12 C11 C13 119.96(14) . .
C10 C11 C13 120.05(15) . .
C11 C12 C7 119.65(15) . .
C11 C12 H12 120.2 . .
C7 C12 H12 120.2 . .
O4 C13 O5 123.39(15) . .
O4 C13 C11 120.31(15) . .
O5 C13 C11 116.17(14) . .
O3 C14 O2 122.41(15) . .
O3 C14 C9 121.55(15) . .
O2 C14 C9 115.97(15) . .
N3 C15 C16 123.05(16) . .
N3 C15 H15 118.5 . .
C16 C15 H15 118.5 . .
C15 C16 C17 119.71(17) . .
C15 C16 H16 120.1 . .
C17 C16 H16 120.1 . .
C18 C17 C16 117.28(15) . .
C18 C17 C22 122.44(16) . .
C16 C17 C22 120.25(16) . .
C17 C18 C19 119.88(17) . .
C17 C18 H18 120.1 . .
C19 C18 H18 120.1 . .
N3 C19 C18 122.60(17) . .
N3 C19 H19 118.7 . .
C18 C19 H19 118.7 . .
N4 C20 C21 123.25(18) . .
N4 C20 H20 118.4 . .
C21 C20 H20 118.4 . .
C20 C21 C22 119.29(18) . .
C20 C21 H21 120.4 . .
C22 C21 H21 120.4 . .
C23 C22 C21 117.79(16) . .
C23 C22 C17 120.98(16) . .
C21 C22 C17 121.14(16) . .
C22 C23 C24 118.64(18) . .
C22 C23 H23 120.7 . .
C24 C23 H23 120.7 . .
N4 C24 C23 123.93(19) . .
N4 C24 H24 118.0 . .
C23 C24 H24 118.0 . .
N2 N1 C4 113.41(16) . .
N1 N2 C7 114.79(15) . .
C19 N3 C15 117.43(15) . .
C19 N3 Zn1 126.76(12) . .
C15 N3 Zn1 115.76(11) . .
C24 N4 C20 117.03(16) . .
C1 O1 H1 109.5 . .
C14 O2 Zn1 115.54(12) . 1_655
C13 O5 Zn1 116.24(11) . .
Zn1 O6 H6A 110.7 . .
Zn1 O6 H6B 110.5 . .
H6A O6 H6B 108.2 . .
H7A O7 H7B 106(2) . .
O2 Zn1 O5 116.20(7) 1_455 .
O2 Zn1 O6 109.02(6) 1_455 .
O5 Zn1 O6 105.06(6) . .
O2 Zn1 N3 125.28(6) 1_455 .
O5 Zn1 N3 97.28(7) . .
O6 Zn1 N3 101.52(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.361(3) .
C1 C6 1.381(4) .
C1 C2 1.391(3) .
C2 C3 1.378(3) .
C2 H2 0.9300 .
C3 C4 1.395(3) .
C3 H3 0.9300 .
C4 C5 1.389(3) .
C4 N1 1.430(2) .
C5 C6 1.396(3) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 C8 1.394(2) .
C7 C12 1.396(2) .
C7 N2 1.432(2) .
C8 C9 1.400(2) .
C8 H8 0.9300 .
C9 C10 1.394(2) .
C9 C14 1.509(2) .
C10 C11 1.399(2) .
C10 H10 0.9300 .
C11 C12 1.397(2) .
C11 C13 1.506(2) .
C12 H12 0.9300 .
C13 O4 1.242(2) .
C13 O5 1.281(2) .
C14 O3 1.235(2) .
C14 O2 1.286(2) .
C15 N3 1.343(2) .
C15 C16 1.380(2) .
C15 H15 0.9300 .
C16 C17 1.388(2) .
C16 H16 0.9300 .
C17 C18 1.387(3) .
C17 C22 1.493(2) .
C18 C19 1.387(3) .
C18 H18 0.9300 .
C19 N3 1.342(2) .
C19 H19 0.9300 .
C20 N4 1.337(3) .
C20 C21 1.385(3) .
C20 H20 0.9300 .
C21 C22 1.389(3) .
C21 H21 0.9300 .
C22 C23 1.386(3) .
C23 C24 1.390(3) .
C23 H23 0.9300 .
C24 N4 1.329(3) .
C24 H24 0.9300 .
N1 N2 1.254(2) .
N3 Zn1 2.0462(17) .
O1 H1 0.8200 .
O2 Zn1 1.9449(16) 1_655
O5 Zn1 1.9484(16) .
O6 Zn1 2.0014(17) .
O6 H6A 0.8685 .
O6 H6B 0.8684 .
O7 H7A 0.858(10) .
O7 H7B 0.852(10) .
Zn1 O2 1.9449(16) 1_455
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C15 H15 O5 0.93 2.59 3.086(3) 114.1 .
C19 H19 O3 0.93 2.53 3.259(3) 134.9 1_455
O1 H1 O7 0.82 1.86 2.623(3) 154.2 .
O6 H6A N4 0.87 1.86 2.719(2) 171.2 1_444
O6 H6B O3 0.87 1.80 2.659(2) 170.9 2_667
O7 H7A O2 0.858(10) 2.048(15) 2.872(3) 161(3) 1_444
O7 H7B O4 0.852(10) 1.901(13) 2.735(3) 166(4) 2
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
O1 C1 C2 C3 179.6(3) .
C6 C1 C2 C3 -0.8(4) .
C1 C2 C3 C4 0.5(4) .
C2 C3 C4 C5 -0.4(4) .
C2 C3 C4 N1 179.1(2) .
C3 C4 C5 C6 0.7(4) .
N1 C4 C5 C6 -178.8(2) .
O1 C1 C6 C5 -179.3(2) .
C2 C1 C6 C5 1.1(4) .
C4 C5 C6 C1 -1.0(4) .
C12 C7 C8 C9 2.8(2) .
N2 C7 C8 C9 -178.98(15) .
C7 C8 C9 C10 -3.7(2) .
C7 C8 C9 C14 172.12(15) .
C8 C9 C10 C11 1.9(2) .
C14 C9 C10 C11 -173.83(15) .
C9 C10 C11 C12 0.6(2) .
C9 C10 C11 C13 178.67(15) .
C10 C11 C12 C7 -1.5(2) .
C13 C11 C12 C7 -179.53(15) .
C8 C7 C12 C11 -0.2(2) .
N2 C7 C12 C11 -178.26(15) .
C12 C11 C13 O4 8.6(2) .
C10 C11 C13 O4 -169.38(16) .
C12 C11 C13 O5 -175.42(15) .
C10 C11 C13 O5 6.6(2) .
C10 C9 C14 O3 5.6(3) .
C8 C9 C14 O3 -170.15(17) .
C10 C9 C14 O2 -177.36(15) .
C8 C9 C14 O2 6.9(2) .
N3 C15 C16 C17 -1.6(3) .
C15 C16 C17 C18 1.2(3) .
C15 C16 C17 C22 -176.97(17) .
C16 C17 C18 C19 0.5(3) .
C22 C17 C18 C19 178.7(2) .
C17 C18 C19 N3 -2.1(4) .
N4 C20 C21 C22 -1.3(4) .
C20 C21 C22 C23 1.4(3) .
C20 C21 C22 C17 178.08(19) .
C18 C17 C22 C23 -44.4(3) .
C16 C17 C22 C23 133.7(2) .
C18 C17 C22 C21 139.0(2) .
C16 C17 C22 C21 -42.9(3) .
C21 C22 C23 C24 0.4(3) .
C17 C22 C23 C24 -176.34(19) .
C22 C23 C24 N4 -2.5(4) .
C5 C4 N1 N2 168.71(18) .
C3 C4 N1 N2 -10.7(3) .
C4 N1 N2 C7 178.11(14) .
C8 C7 N2 N1 157.23(16) .
C12 C7 N2 N1 -24.7(2) .
C18 C19 N3 C15 1.8(3) .
C18 C19 N3 Zn1 -175.51(17) .
C16 C15 N3 C19 0.1(3) .
C16 C15 N3 Zn1 177.68(15) .
C23 C24 N4 C20 2.6(4) .
C21 C20 N4 C24 -0.7(3) .
O3 C14 O2 Zn1 22.9(2) 1_655
C9 C14 O2 Zn1 -154.15(12) 1_655
O4 C13 O5 Zn1 1.2(2) .
C11 C13 O5 Zn1 -174.55(11) .
