#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:01:10 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301838 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/05/4320586.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_4320586
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
_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                 104.099(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1965(9)
_cell_length_b                   12.9185(12)
_cell_length_c                   12.7306(12)
_cell_measurement_reflns_used    6655
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.998
_cell_measurement_theta_min      2.282
_cell_volume                     1466.9(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1080
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_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            11849
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.60
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2593
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0486
_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)+(0.0803P)²+0.1450P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1495
_reflns_number_gt                2090
_reflns_number_total             2593
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010574k_3.cif
_cod_data_source_block           rs57t
_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               4320586
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 1.02589(18) 0.79603(13) 0.09528(13) 0.0525(4) Uani 1 1 d . . .
C2 C 1.1309(2) 0.87439(15) 0.16522(14) 0.0625(5) Uani 1 1 d . . .
H2A H 1.2336 0.8503 0.1778 0.065(5) Uiso 1 1 calc R . .
H2B H 1.1236 0.9402 0.1277 0.065(5) Uiso 1 1 calc R . .
C3 C 1.0742(3) 0.99270(16) 0.29151(18) 0.0776(6) Uani 1 1 d . . .
H3A H 0.9940 1.0239 0.2368 0.146(12) Uiso 1 1 calc R . .
H3B H 1.1658 1.0310 0.2943 0.097(7) Uiso 1 1 calc R . .
C4 C 1.0367(2) 0.99610(14) 0.39988(15) 0.0621(5) Uani 1 1 d . . .
C5 C 0.9018(3) 0.9639(3) 0.4115(2) 0.1050(10) Uani 1 1 d . . .
H5 H 0.8315 0.9391 0.3513 0.120(9) Uiso 1 1 calc R . .
C6 C 1.1342(3) 1.0330(2) 0.4896(2) 0.1005(9) Uani 1 1 d . . .
H6 H 1.2276 1.0567 0.4843 0.109(8) Uiso 1 1 calc R . .
C11 C 1.0521(2) 0.66699(16) 0.24894(13) 0.0612(5) Uani 1 1 d . . .
H11 H 1.0695 0.7121 0.3076 0.073(6) Uiso 1 1 calc R . .
C12 C 1.0345(2) 0.56316(17) 0.25199(15) 0.0715(6) Uani 1 1 d . . .
H12 H 1.0382 0.5223 0.3127 0.088(7) Uiso 1 1 calc R . .
C13 C 1.0099(3) 0.53084(17) 0.14581(16) 0.0737(6) Uani 1 1 d . . .
H13 H 0.9944 0.4622 0.1239 0.083(6) Uiso 1 1 calc R . .
C21 C 0.7469(2) 0.77181(17) 0.07862(15) 0.0676(5) Uani 1 1 d . . .
H21 H 0.7435 0.7012 0.0920 0.069(6) Uiso 1 1 calc R . .
C22 C 0.6288(2) 0.8383(2) 0.05561(16) 0.0770(6) Uani 1 1 d . . .
H22 H 0.5284 0.8229 0.0501 0.089(7) Uiso 1 1 calc R . .
C23 C 0.6900(2) 0.93406(19) 0.04205(16) 0.0757(6) Uani 1 1 d . . .
H23 H 0.6343 0.9946 0.0258 0.091(7) Uiso 1 1 calc R . .
C31 C 0.9688(3) 0.77123(17) -0.10704(15) 0.0742(6) Uani 1 1 d . . .
H31 H 0.8651 0.7646 -0.1217 0.105(8) Uiso 1 1 calc R . .
C32 C 1.0535(3) 0.76400(19) -0.17937(17) 0.0865(7) Uani 1 1 d . . .
H32 H 1.0214 0.7519 -0.2534 0.096(7) Uiso 1 1 calc R . .
C33 C 1.1966(3) 0.7784(2) -0.1199(2) 0.0900(7) Uani 1 1 d . . .
H33 H 1.2795 0.7775 -0.1496 0.123(10) Uiso 1 1 calc R . .
N11 N 1.0109(2) 0.60881(12) 0.07883(12) 0.0672(5) Uani 1 1 d . . .
N12 N 1.03969(15) 0.69261(11) 0.14400(10) 0.0533(4) Uani 1 1 d . . .
N21 N 0.83679(19) 0.92924(13) 0.05493(13) 0.0685(5) Uani 1 1 d . . .
N22 N 0.87024(15) 0.82879(12) 0.07815(10) 0.0550(4) Uani 1 1 d . . .
N31 N 1.20600(19) 0.79369(15) -0.01538(15) 0.0797(5) Uani 1 1 d . . .
N32 N 1.06189(17) 0.78988(11) -0.00970(11) 0.0571(4) Uani 1 1 d . . .
O1 O 1.09299(17) 0.88768(10) 0.26527(10) 0.0703(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
N32 C1 N22 108.26(13) . . ?
N32 C1 N12 108.86(13) . . ?
N22 C1 N12 107.98(13) . . ?
N32 C1 C2 108.57(14) . . ?
N22 C1 C2 110.71(14) . . ?
N12 C1 C2 112.36(14) . . ?
O1 C2 C1 110.28(14) . . ?
O1 C3 C4 108.22(16) . . ?
C5 C4 C6 116.96(19) . . ?
C5 C4 C3 120.94(19) . . ?
C6 C4 C3 122.09(19) . . ?
C4 C5 C6 121.5(2) . 3_776 ?
C4 C6 C5 121.5(2) . 3_776 ?
C12 C11 N12 106.79(16) . . ?
C11 C12 C13 105.31(17) . . ?
N11 C13 C12 112.11(19) . . ?
N22 C21 C22 106.4(2) . . ?
C21 C22 C23 105.24(19) . . ?
N21 C23 C22 112.10(19) . . ?
N32 C31 C32 107.4(2) . . ?
C31 C32 C33 104.60(19) . . ?
N31 C33 C32 113.33(19) . . ?
C13 N11 N12 104.23(15) . . ?
N11 N12 C11 111.53(14) . . ?
N11 N12 C1 119.15(13) . . ?
C11 N12 C1 128.20(14) . . ?
C23 N21 N22 104.12(16) . . ?
N21 N22 C21 112.16(15) . . ?
N21 N22 C1 118.37(14) . . ?
C21 N22 C1 129.44(16) . . ?
C33 N31 N32 102.93(18) . . ?
C31 N32 N31 111.78(16) . . ?
C31 N32 C1 128.30(16) . . ?
N31 N32 C1 119.65(14) . . ?
C2 O1 C3 113.59(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 N32 1.4553(19) . ?
C1 N22 1.457(2) . ?
C1 N12 1.465(2) . ?
C1 C2 1.527(2) . ?
C2 O1 1.411(2) . ?
C3 O1 1.418(2) . ?
C3 C4 1.502(3) . ?
C4 C5 1.350(3) . ?
C4 C6 1.355(3) . ?
C5 C6 1.379(3) 3_776 ?
C6 C5 1.379(3) 3_776 ?
C11 C12 1.353(3) . ?
C11 N12 1.354(2) . ?
C12 C13 1.380(3) . ?
C13 N11 1.321(2) . ?
C21 N22 1.354(2) . ?
C21 C22 1.360(3) . ?
C22 C23 1.387(3) . ?
C23 N21 1.321(3) . ?
C31 N32 1.345(2) . ?
C31 C32 1.346(3) . ?
C32 C33 1.361(4) . ?
C33 N31 1.327(3) . ?
N11 N12 1.350(2) . ?
N21 N22 1.350(2) . ?
N31 N32 1.346(2) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 12057030
