#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/05/4320585.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_4320585
loop_
_publ_author_name
'Daniel L. Reger'
'Terri D. Wright'
'Radu F. Semeniuc'
'T. Christian Grattan'
'Mark D. Smith'
_publ_section_title
;
 Supramolecular Structures of Cadmium(II) Coordination Polymers: A New
 Class of Ligands Formed by Linking Tripodal Tris(pyrazolyl)methane Units
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6212
_journal_page_last               6219
_journal_paper_doi               10.1021/ic010574k
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C30 H30 N12 O2'
_chemical_formula_weight         590.66
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.134(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3157(13)
_cell_length_b                   8.5880(6)
_cell_length_c                   21.9227(17)
_cell_measurement_reflns_used    5889
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.898
_cell_measurement_theta_min      2.3715
_cell_volume                     3023.9(4)
_computing_cell_refinement       'SAINT+ NT V6.02a (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.619 (Bruker, 2000)'
_computing_data_reduction        'SAINT+ NT V6.02a'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17712
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.167
_refine_diff_density_min         -0.143
_refine_diff_density_rms         0.026
_refine_ls_extinction_coef       0.0016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         5357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0500P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1119
_reflns_number_gt                3246
_reflns_number_total             5357
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010574k_1.cif
_cod_data_source_block           rs561t
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4320585
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.71490(10) 0.7942(2) 0.06003(8) 0.0534(5) Uani 1 1 d . . .
C2 C 1.06169(12) 0.2085(2) 0.23356(9) 0.0618(5) Uani 1 1 d . . .
C11 C 0.64021(17) 0.6183(2) 0.12315(13) 0.0848(7) Uani 1 1 d . . .
H11 H 0.5871 0.6205 0.0993 0.136(11) Uiso 1 1 calc R . .
C12 C 0.6628(2) 0.5480(3) 0.17856(16) 0.1123(10) Uani 1 1 d . . .
H12 H 0.6290 0.4930 0.2009 0.142(11) Uiso 1 1 calc R . .
C13 C 0.7469(3) 0.5753(3) 0.19482(13) 0.1157(10) Uani 1 1 d . . .
H13 H 0.7794 0.5383 0.2310 0.157(12) Uiso 1 1 calc R . .
C21 C 0.67804(19) 0.9957(3) 0.13330(12) 0.1115(10) Uani 1 1 d . . .
H21 H 0.6570 0.9316 0.1611 0.125(10) Uiso 1 1 calc R . .
C22 C 0.6831(2) 1.1529(3) 0.13537(15) 0.1250(12) Uani 1 1 d . . .
H22 H 0.6680 1.2185 0.1653 0.146(11) Uiso 1 1 calc R . .
C23 C 0.71538(15) 1.1950(3) 0.08404(16) 0.0955(8) Uani 1 1 d . . .
H23 H 0.7253 1.2973 0.0734 0.113(9) Uiso 1 1 calc R . .
C31 C 0.63610(14) 0.6580(3) -0.03428(10) 0.0815(7) Uani 1 1 d . . .
H31 H 0.6772 0.5908 -0.0430 0.094(8) Uiso 1 1 calc R . .
C32 C 0.55660(16) 0.6640(3) -0.06380(12) 0.0983(8) Uani 1 1 d . . .
H32 H 0.5314 0.6028 -0.0969 0.119(9) Uiso 1 1 calc R . .
C33 C 0.52072(16) 0.7803(3) -0.03439(12) 0.1010(8) Uani 1 1 d . . .
H33 H 0.4653 0.8102 -0.0453 0.121(9) Uiso 1 1 calc R . .
C41 C 1.18339(17) 0.0850(3) 0.19469(12) 0.0932(7) Uani 1 1 d . . .
H41 H 1.1727 -0.0200 0.2002 0.107(8) Uiso 1 1 calc R . .
C42 C 1.24926(19) 0.1450(3) 0.17299(13) 0.1060(9) Uani 1 1 d . . .
H42 H 1.2923 0.0903 0.1600 0.130(10) Uiso 1 1 calc R . .
C43 C 1.23928(15) 0.3013(3) 0.17411(10) 0.0809(6) Uani 1 1 d . . .
H43 H 1.2763 0.3722 0.1618 0.079(7) Uiso 1 1 calc R . .
C51 C 0.96395(13) -0.0154(3) 0.19606(10) 0.0742(6) Uani 1 1 d . . .
H51 H 0.9289 0.0327 0.1635 0.089(7) Uiso 1 1 calc R . .
C52 C 0.96017(14) -0.1653(3) 0.21372(10) 0.0795(6) Uani 1 1 d . . .
H52 H 0.9224 -0.2409 0.1962 0.090(7) Uiso 1 1 calc R . .
C53 C 1.02391(15) -0.1821(3) 0.26296(12) 0.0864(7) Uani 1 1 d . . .
H53 H 1.0363 -0.2749 0.2845 0.104(8) Uiso 1 1 calc R . .
C61 C 1.15900(19) 0.2468(3) 0.33590(11) 0.0875(7) Uani 1 1 d . . .
H61 H 1.2075 0.2041 0.3263 0.156(14) Uiso 1 1 calc R . .
C62 C 1.1477(2) 0.3047(3) 0.39137(12) 0.1098(10) Uani 1 1 d . . .
H62 H 1.1870 0.3113 0.4276 0.130(10) Uiso 1 1 calc R . .
C63 C 1.0665(2) 0.3514(4) 0.38291(13) 0.1179(10) Uani 1 1 d . . .
H63 H 1.0421 0.3951 0.4141 0.149(11) Uiso 1 1 calc R . .
C70 C 0.79772(11) 0.7803(2) 0.03815(10) 0.0653(5) Uani 1 1 d . . .
H70A H 0.7980 0.8472 0.0025 0.077(6) Uiso 1 1 calc R . .
H70B H 0.8424 0.8133 0.0708 0.079(6) Uiso 1 1 calc R . .
C71 C 0.88520(12) 0.6081(2) -0.00270(10) 0.0658(5) Uani 1 1 d . . .
H71A H 0.9323 0.6462 0.0268 0.065(6) Uiso 1 1 calc R . .
H71B H 0.8814 0.6681 -0.0406 0.074(6) Uiso 1 1 calc R . .
C72 C 0.89667(10) 0.4397(2) -0.01569(10) 0.0581(5) Uani 1 1 d . . .
C73 C 0.91536(11) 0.3301(2) 0.03203(9) 0.0574(5) Uani 1 1 d . . .
C74 C 0.92287(12) 0.1756(2) 0.01674(11) 0.0686(6) Uani 1 1 d . . .
H74 H 0.9347 0.1019 0.0481 0.070(6) Uiso 1 1 calc R . .
C75 C 0.91320(13) 0.1283(3) -0.04407(12) 0.0790(6) Uani 1 1 d . . .
H75 H 0.9179 0.0234 -0.0535 0.091(7) Uiso 1 1 calc R . .
C76 C 0.89665(13) 0.2359(3) -0.09085(11) 0.0796(6) Uani 1 1 d . . .
H76 H 0.8914 0.2048 -0.1320 0.095(8) Uiso 1 1 calc R . .
C77 C 0.88797(12) 0.3895(3) -0.07647(10) 0.0720(6) Uani 1 1 d . . .
H77 H 0.8759 0.4619 -0.1083 0.078(6) Uiso 1 1 calc R . .
C78 C 0.92750(13) 0.3803(2) 0.09849(9) 0.0700(6) Uani 1 1 d . . .
H78A H 0.9482 0.4864 0.1023 0.112(8) Uiso 1 1 calc R . .
H78B H 0.8747 0.3773 0.1130 0.093(7) Uiso 1 1 calc R . .
C79 C 0.99849(14) 0.3212(2) 0.19807(9) 0.0715(6) Uani 1 1 d . . .
H79A H 0.9466 0.3156 0.2138 0.077(6) Uiso 1 1 calc R . .
H79B H 1.0194 0.4269 0.2032 0.076(6) Uiso 1 1 calc R . .
N11 N 0.77621(13) 0.6599(2) 0.15322(10) 0.0972(7) Uani 1 1 d . . .
N12 N 0.70873(10) 0.68443(17) 0.10910(7) 0.0604(4) Uani 1 1 d . . .
N21 N 0.73048(11) 1.0729(2) 0.05190(10) 0.0899(6) Uani 1 1 d . . .
N22 N 0.70890(10) 0.95032(18) 0.08393(8) 0.0652(4) Uani 1 1 d . . .
N31 N 0.57303(11) 0.8444(2) 0.01068(9) 0.0839(6) Uani 1 1 d . . .
N32 N 0.64509(9) 0.76769(17) 0.01027(7) 0.0586(4) Uani 1 1 d . . .
N41 N 1.17143(12) 0.34137(19) 0.19455(9) 0.0803(5) Uani 1 1 d . . .
N42 N 1.13670(10) 0.20443(18) 0.20662(7) 0.0597(4) Uani 1 1 d . . .
N51 N 1.06561(11) -0.0518(2) 0.27629(9) 0.0895(6) Uani 1 1 d . . .
N52 N 1.02771(10) 0.05168(18) 0.23417(7) 0.0651(4) Uani 1 1 d . . .
N61 N 1.02572(13) 0.3280(3) 0.32512(10) 0.1046(7) Uani 1 1 d . . .
N62 N 1.08447(12) 0.26417(19) 0.29714(8) 0.0719(5) Uani 1 1 d . . .
O1 O 0.81053(7) 0.62458(13) 0.02199(6) 0.0664(4) Uani 1 1 d . . .
O2 O 0.98507(8) 0.27956(14) 0.13477(6) 0.0718(4) Uani 1 1 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'
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
_geom_angle_publ_flag
N12 C1 N22 108.43(15) . . ?
N12 C1 N32 108.00(14) . . ?
N22 C1 N32 108.85(13) . . ?
N12 C1 C70 111.50(15) . . ?
N22 C1 C70 107.92(15) . . ?
N32 C1 C70 112.05(16) . . ?
N42 C2 N52 109.33(16) . . ?
N42 C2 N62 107.81(15) . . ?
N52 C2 N62 109.12(15) . . ?
N42 C2 C79 110.56(17) . . ?
N52 C2 C79 111.53(16) . . ?
N62 C2 C79 108.40(16) . . ?
N12 C11 C12 106.9(3) . . ?
C11 C12 C13 105.1(3) . . ?
N11 C13 C12 112.4(3) . . ?
N22 C21 C22 106.8(3) . . ?
C21 C22 C23 105.4(3) . . ?
N21 C23 C22 111.4(2) . . ?
C32 C31 N32 107.2(2) . . ?
C31 C32 C33 104.8(2) . . ?
N31 C33 C32 112.6(2) . . ?
N42 C41 C42 107.1(2) . . ?
C41 C42 C43 105.4(3) . . ?
N41 C43 C42 112.2(2) . . ?
N52 C51 C52 107.46(19) . . ?
C51 C52 C53 105.09(19) . . ?
N51 C53 C52 112.2(2) . . ?
C62 C61 N62 105.8(3) . . ?
C61 C62 C63 105.5(3) . . ?
N61 C63 C62 113.2(3) . . ?
O1 C70 C1 109.53(15) . . ?
O1 C71 C72 108.25(15) . . ?
C77 C72 C73 118.82(18) . . ?
C77 C72 C71 119.38(18) . . ?
C73 C72 C71 121.80(19) . . ?
C74 C73 C72 118.81(19) . . ?
C74 C73 C78 120.71(18) . . ?
C72 C73 C78 120.48(17) . . ?
C75 C74 C73 121.3(2) . . ?
C76 C75 C74 120.0(2) . . ?
C77 C76 C75 119.5(2) . . ?
C76 C77 C72 121.6(2) . . ?
O2 C78 C73 109.37(16) . . ?
O2 C79 C2 108.37(16) . . ?
C13 N11 N12 103.5(2) . . ?
C11 N12 N11 112.25(19) . . ?
C11 N12 C1 128.17(18) . . ?
N11 N12 C1 118.72(17) . . ?
C23 N21 N22 104.7(2) . . ?
C21 N22 N21 111.51(19) . . ?
C21 N22 C1 128.6(2) . . ?
N21 N22 C1 119.66(18) . . ?
C33 N31 N32 104.07(18) . . ?
C31 N32 N31 111.26(16) . . ?
C31 N32 C1 128.81(16) . . ?
N31 N32 C1 119.24(15) . . ?
C43 N41 N42 104.29(18) . . ?
C41 N42 N41 110.99(19) . . ?
C41 N42 C2 130.70(19) . . ?
N41 N42 C2 118.14(16) . . ?
C53 N51 N52 104.55(17) . . ?
C51 N52 N51 110.75(16) . . ?
C51 N52 C2 130.12(17) . . ?
N51 N52 C2 119.03(15) . . ?
C63 N61 N62 102.6(2) . . ?
N61 N62 C61 113.0(2) . . ?
N61 N62 C2 119.21(18) . . ?
C61 N62 C2 127.5(2) . . ?
C70 O1 C71 111.38(13) . . ?
C79 O2 C78 111.75(14) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N12 1.447(2) . ?
C1 N22 1.449(2) . ?
C1 N32 1.450(2) . ?
C1 C70 1.516(2) . ?
C2 N42 1.450(2) . ?
C2 N52 1.458(2) . ?
C2 N62 1.458(2) . ?
C2 C79 1.524(3) . ?
C11 N12 1.337(3) . ?
C11 C12 1.349(3) . ?
C12 C13 1.375(4) . ?
C13 N11 1.319(3) . ?
C21 N22 1.330(3) . ?
C21 C22 1.353(3) . ?
C22 C23 1.372(4) . ?
C23 N21 1.310(3) . ?
C31 C32 1.345(3) . ?
C31 N32 1.346(2) . ?
C32 C33 1.375(3) . ?
C33 N31 1.308(3) . ?
C41 N42 1.331(3) . ?
C41 C42 1.351(3) . ?
C42 C43 1.353(3) . ?
C43 N41 1.311(3) . ?
C51 N52 1.344(2) . ?
C51 C52 1.349(3) . ?
C52 C53 1.368(3) . ?
C53 N51 1.316(2) . ?
C61 C62 1.356(4) . ?
C61 N62 1.364(3) . ?
C62 C63 1.365(4) . ?
C63 N61 1.339(3) . ?
C70 O1 1.408(2) . ?
C71 O1 1.425(2) . ?
C71 C72 1.492(2) . ?
C72 C77 1.384(3) . ?
C72 C73 1.400(2) . ?
C73 C74 1.380(2) . ?
C73 C78 1.499(3) . ?
C74 C75 1.376(3) . ?
C75 C76 1.372(3) . ?
C76 C77 1.370(3) . ?
C78 O2 1.415(2) . ?
C79 O2 1.412(2) . ?
N11 N12 1.348(2) . ?
N21 N22 1.346(2) . ?
N31 N32 1.349(2) . ?
N41 N42 1.352(2) . ?
N51 N52 1.351(2) . ?
N61 N62 1.343(2) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30660928
