#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:24:26 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179629 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/93/4509361.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4509361
loop_
_publ_author_name
'Hunger, Jens'
'Krautscheid, Harald'
'Sieler, Joachim'
_publ_section_title
;
 Hydrothermal Synthesis and Structure of Coordination Polymers by
 Combination of Bipyrazole and Aromatic Dicarboxylate Ligands
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4613
_journal_paper_doi               10.1021/cg801282r
_journal_volume                  9
_journal_year                    2009
_chemical_formula_moiety         'C18 H20 Cd N4 O6'
_chemical_formula_sum            'C18 H20 Cd N4 O6'
_chemical_formula_weight         500.78
_chemical_name_systematic
;
catena-((μ₃-5-hydroxy-benzene-1,3-dicarboxylato)-aqua-(3,3',5,5'-
tetramethyl-4,4'-bipyrazole)-cadmium(ii))
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.421(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3578(8)
_cell_length_b                   18.3162(8)
_cell_length_c                   7.7720(5)
_cell_measurement_reflns_used    25900
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      29.63
_cell_measurement_theta_min      3.255
_cell_volume                     1881.03(19)
_computing_cell_refinement       'RECIPE (Stoe & Cie, 2002)'
_computing_data_collection       'WinXpose (Stoe & Cie, 2002)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 and DIAMOND'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe IPDS-2T'
_diffrn_measurement_method       'ω-scan and φ-scan'
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18066
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         3.28
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_T_max  0.7641
_exptl_absorpt_correction_T_min  0.6565
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
[X-RED32 (Stoe & Cie, 2001);
crystal description using FACEIT (Stoe & Cie, 2002);
optimization using equivalent reflections
(X-SHAPE; Stoe & Cie, 1999)]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0159
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0283P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0388
_refine_ls_wR_factor_ref         0.0394
_reflns_number_gt                3947
_reflns_number_total             4540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg801282rsup1.cif
_cod_data_source_block           9
_cod_original_cell_volume        1881.03(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4509361
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
C1 C 0.72268(10) -0.16597(7) 0.77119(17) 0.0093(2) Uani 1 1 d .
C2 C 0.81536(10) -0.13055(7) 0.81175(17) 0.0092(2) Uani 1 1 d .
C3 C 0.79389(10) -0.06707(7) 0.90260(17) 0.0103(2) Uani 1 1 d .
C4 C 0.69422(10) -0.23406(8) 0.67104(18) 0.0124(3) Uani 1 1 d .
H4A H 0.6781 -0.2704 0.7466 0.019 Uiso 1 1 calc R
H4B H 0.7485 -0.2495 0.6168 0.019 Uiso 1 1 calc R
H4C H 0.6382 -0.22495 0.5869 0.019 Uiso 1 1 calc R
C5 C 0.86392(10) -0.00630(8) 0.96588(19) 0.0142(3) Uani 1 1 d .
H5A H 0.8297 0.0382 0.9484 0.021 Uiso 1 1 calc R
H5B H 0.9191 -0.0064 0.9045 0.021 Uiso 1 1 calc R
H5C H 0.8869 -0.0126 1.0845 0.021 Uiso 1 1 calc R
C6 C 1.00516(10) -0.15599(7) 0.88205(18) 0.0100(2) Uani 1 1 d .
C7 C 0.91562(10) -0.14815(7) 0.76612(18) 0.0096(2) Uani 1 1 d .
C8 C 0.94629(10) -0.14774(7) 0.59993(18) 0.0108(3) Uani 1 1 d .
C9 C 1.02395(11) -0.16230(8) 1.07540(18) 0.0141(3) Uani 1 1 d .
H9A H 1.0934 -0.1749 1.1123 0.021 Uiso 1 1 calc R
H9B H 0.9811 -0.1995 1.1119 0.021 Uiso 1 1 calc R
H9C H 1.0094 -0.1166 1.1263 0.021 Uiso 1 1 calc R
C10 C 0.88025(11) -0.14395(9) 0.42778(19) 0.0165(3) Uani 1 1 d .
H10A H 0.8988 -0.1023 0.3645 0.025 Uiso 1 1 calc R
H10B H 0.8109 -0.1395 0.4452 0.025 Uiso 1 1 calc R
H10C H 0.8886 -0.1875 0.3630 0.025 Uiso 1 1 calc R
C11 C 0.47647(10) 0.08741(7) 0.72097(17) 0.0103(2) Uani 1 1 d .
C12 C 0.56581(10) 0.12877(7) 0.67422(17) 0.0098(2) Uani 1 1 d .
C13 C 0.56007(10) 0.20455(7) 0.65908(17) 0.0098(2) Uani 1 1 d .
C14 C 0.64180(10) 0.24354(7) 0.61469(17) 0.0092(2) Uani 1 1 d .
C15 C 0.63606(10) 0.32510(7) 0.60177(17) 0.0095(2) Uani 1 1 d .
C16 C 0.72848(10) 0.20684(7) 0.57992(17) 0.0097(2) Uani 1 1 d .
C17 C 0.73362(10) 0.13110(7) 0.59452(17) 0.0091(2) Uani 1 1 d .
C18 C 0.65294(10) 0.09209(7) 0.64422(17) 0.0101(2) Uani 1 1 d .
N1 N 0.69616(8) -0.06420(6) 0.91932(15) 0.0104(2) Uani 1 1 d .
N2 N 0.65392(9) -0.12491(6) 0.83818(15) 0.0101(2) Uani 1 1 d .
N3 N 1.04696(9) -0.15390(6) 0.61179(15) 0.0117(2) Uani 1 1 d .
N4 N 1.08062(9) -0.15898(6) 0.78547(15) 0.0109(2) Uani 1 1 d .
O1 O 0.49605(7) 0.03204(5) 0.82390(12) 0.01051(18) Uani 1 1 d .
O2 O 0.39060(8) 0.10763(6) 0.65810(15) 0.0163(2) Uani 1 1 d .
O3 O 0.71333(7) 0.36033(5) 0.57038(13) 0.01122(19) Uani 1 1 d .
O4 O 0.55517(7) 0.35751(5) 0.62084(14) 0.0132(2) Uani 1 1 d .
O5 O 0.81553(7) 0.09198(5) 0.56122(13) 0.01124(19) Uani 1 1 d .
O6 O 0.74092(8) -0.00295(6) 1.29595(14) 0.0138(2) Uani 1 1 d .
Cd1 Cd 0.627253(7) 0.027826(5) 1.059266(12) 0.00829(4) Uani 1 1 d .
H2N H 0.5945(16) -0.1323(11) 0.837(3) 0.020(5) Uiso 1 1 d .
H4N H 1.1457(15) -0.1578(10) 0.825(2) 0.015(4) Uiso 1 1 d .
H5O H 0.8605(17) 0.1180(13) 0.518(3) 0.034(6) Uiso 1 1 d .
H6A H 0.7122(16) -0.0362(12) 1.331(3) 0.021(5) Uiso 1 1 d .
H6B H 0.7597(18) 0.0245(13) 1.375(3) 0.035(6) Uiso 1 1 d .
H13 H 0.5030 0.2286 0.681 0.014 Uiso 1 1 calc R
H16 H 0.7824 0.2325 0.549 0.017 Uiso 1 1 calc R
H18 H 0.6568 0.0422 0.657 0.019 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'
Cd Cd -0.8075 1.2024 '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
N2 C1 C2 106.61(12) . .
N2 C1 C4 122.15(12) . .
C2 C1 C4 131.21(12) . .
C1 C2 C3 104.96(12) . .
C1 C2 C7 130.86(12) . .
C3 C2 C7 124.07(12) . .
N1 C3 C2 110.81(12) . .
N1 C3 C5 121.01(12) . .
C2 C3 C5 128.08(12) . .
C1 C4 H4A 109.5 . .
C1 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C1 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C3 C5 H5A 109.5 . .
C3 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C3 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
N4 C6 C7 106.60(12) . .
N4 C6 C9 122.05(12) . .
C7 C6 C9 131.34(13) . .
C6 C7 C8 104.79(12) . .
C6 C7 C2 126.27(12) . .
C8 C7 C2 128.05(12) . .
N3 C8 C7 111.09(12) . .
N3 C8 C10 121.42(12) . .
C7 C8 C10 127.46(12) . .
C6 C9 H9A 109.5 . .
C6 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C6 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C8 C10 H10A 109.5 . .
C8 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C8 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
O2 C11 O1 124.82(12) . .
O2 C11 C12 118.52(12) . .
O1 C11 C12 116.66(11) . .
C18 C12 C13 120.21(13) . .
C18 C12 C11 120.67(12) . .
C13 C12 C11 119.12(12) . .
C14 C13 C12 119.81(13) . .
C14 C13 H13 120.2 . .
C12 C13 H13 120.0 . .
C13 C14 C16 120.22(12) . .
C13 C14 C15 119.65(12) . .
C16 C14 C15 120.12(12) . .
O4 C15 O3 121.19(12) . .
O4 C15 C14 119.87(12) . .
O3 C15 C14 118.95(12) . .
O4 C15 Cd1 61.60(7) . 4_565
O3 C15 Cd1 59.65(7) . 4_565
C14 C15 Cd1 176.76(10) . 4_565
C17 C16 C14 119.69(12) . .
C17 C16 H16 119.9 . .
C14 C16 H16 120.5 . .
O5 C17 C16 122.62(12) . .
O5 C17 C18 117.24(12) . .
C16 C17 C18 120.14(12) . .
C12 C18 C17 119.88(12) . .
C12 C18 H18 119.8 . .
C17 C18 H18 120.3 . .
C3 N1 N2 105.58(11) . .
C3 N1 Cd1 123.20(9) . .
N2 N1 Cd1 131.22(9) . .
C1 N2 N1 112.03(11) . .
C1 N2 H2N 128.9(14) . .
N1 N2 H2N 119.0(14) . .
C8 N3 N4 104.85(11) . .
C6 N4 N3 112.66(11) . .
C6 N4 H4N 126.0(12) . .
N3 N4 H4N 120.7(12) . .
C11 O1 Cd1 122.11(8) . 3_657
C11 O1 Cd1 124.68(8) . .
Cd1 O1 Cd1 100.08(4) 3_657 .
C15 O3 Cd1 92.46(8) . 4_565
C15 O4 Cd1 90.74(8) . 4_565
C17 O5 H5O 113.8(15) . .
Cd1 O6 H6A 99.7(15) . .
Cd1 O6 H6B 123.9(16) . .
H6A O6 H6B 109(2) . .
N1 Cd1 O1 101.60(4) . 3_657
N1 Cd1 O6 86.22(4) . .
O1 Cd1 O6 89.68(4) 3_657 .
N1 Cd1 O1 87.70(4) . .
O1 Cd1 O1 79.92(4) 3_657 .
O6 Cd1 O1 166.66(4) . .
N1 Cd1 O3 115.78(4) . 4_566
O1 Cd1 O3 141.82(3) 3_657 4_566
O6 Cd1 O3 85.48(4) . 4_566
O1 Cd1 O3 107.87(3) . 4_566
N1 Cd1 O4 162.13(4) . 4_566
O1 Cd1 O4 90.41(3) 3_657 4_566
O6 Cd1 O4 107.24(4) . 4_566
O1 Cd1 O4 81.37(3) . 4_566
O3 Cd1 O4 55.54(3) 4_566 4_566
N1 Cd1 C15 141.35(4) . 4_566
O1 Cd1 C15 116.79(4) 3_657 4_566
O6 Cd1 C15 97.78(4) . 4_566
O1 Cd1 C15 94.39(4) . 4_566
O3 Cd1 C15 27.89(4) 4_566 4_566
O4 Cd1 C15 27.67(4) 4_566 4_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.3492(17) .
C1 C2 1.3923(18) .
C1 C4 1.4897(18) .
C2 C3 1.4113(18) .
C2 C7 1.4705(18) .
C3 N1 1.3317(17) .
C3 C5 1.4903(19) .
C4 H4A 0.9338 .
C4 H4B 0.9338 .
C4 H4C 0.9338 .
C5 H5A 0.9348 .
C5 H5B 0.9348 .
C5 H5C 0.9348 .
C6 N4 1.3432(18) .
C6 C7 1.3955(18) .
C6 C9 1.4913(19) .
C7 C8 1.4111(19) .
C8 N3 1.3392(18) .
C8 C10 1.4925(19) .
C9 H9A 0.9585 .
C9 H9B 0.9585 .
C9 H9C 0.9585 .
C10 H10A 0.9591 .
C10 H10B 0.9591 .
C10 H10C 0.9591 .
C11 O2 1.2358(17) .
C11 O1 1.2944(16) .
C11 C12 1.5024(18) .
C12 C18 1.3927(19) .
C12 C13 1.3941(19) .
C13 C14 1.3897(18) .
C13 H13 0.918 .
C14 C16 1.3990(19) .
C14 C15 1.4984(19) .
C15 O4 1.2604(16) .
C15 O3 1.2708(16) .
C16 C17 1.3928(19) .
C16 H16 0.92 .
C17 O5 1.3639(16) .
C17 C18 1.3939(18) .
C18 H18 0.920 .
N1 N2 1.3596(16) .
N1 Cd1 2.2725(11) .
N2 H2N 0.80(2) .
N3 N4 1.3620(16) .
N4 H4N 0.878(19) .
O1 Cd1 2.2755(10) 3_657
O1 Cd1 2.3419(9) .
O3 Cd1 2.3446(10) 4_565
O4 Cd1 2.3878(10) 4_565
O5 H5O 0.87(2) .
O6 Cd1 2.2779(10) .
O6 H6A 0.79(2) .
O6 H6B 0.81(3) .
