#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/59/4505903.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_4505903
loop_
_publ_author_name
'Rigby, Nicola'
'Jacobs, Tia'
'Reddy, Jayarama Prakasha'
'Hardie, Michaele J.'
_publ_section_title
;
 Metal Complexes of 2,2′-Bipyridine-4,4′-diamine as
 Metallo-Tectons for Hydrogen Bonded Networks
;
_journal_issue                   4
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1871
_journal_paper_doi               10.1021/cg201512q
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C30 H35.5 Cd Cl2 N12 O2.75'
_chemical_formula_weight         791.50
_chemical_name_systematic
; 
 tris(2,2'-bipyridine-4,4'-diamine)cadmium(II) chloride hydrate
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   31.7204(10)
_cell_length_b                   31.7204(10)
_cell_length_c                   13.7906(6)
_cell_measurement_temperature    150(2)
_cell_volume                     13875.9(9)
_computing_cell_refinement       'APEXII (Bruker, 2004)'
_computing_data_collection       'APEXII (Bruker, 2004)'
_computing_data_reduction        'APEXII (Bruker, 2004)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            49171
_diffrn_reflns_theta_full        20.75
_diffrn_reflns_theta_max         20.75
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  0.9595
_exptl_absorpt_correction_T_min  0.8510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             6456
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.100
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         3604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0796P)²+201.4047P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1546
_reflns_number_gt                2755
_reflns_number_total             3604
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201512q_si_001.cif
_cod_data_source_block           c:
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      I4(1)/a
_cod_original_formula_sum        'C30 H35.50 Cd Cl2 N12 O2.75'
_cod_database_code               4505903
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'
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
Cd1 Cd 0.606281(19) 0.46437(2) 0.46954(5) 0.0290(3) Uani 1 1 d .
N1 N 0.5794(2) 0.5210(2) 0.5565(5) 0.0311(18) Uani 1 1 d .
C1 C 0.5849(3) 0.5284(3) 0.6509(7) 0.039(2) Uani 1 1 d .
H1 H 0.6064 0.5130 0.6835 0.046 Uiso 1 1 calc R
N2 N 0.5549(2) 0.4976(2) 0.3734(5) 0.0301(18) Uani 1 1 d .
C2 C 0.5617(3) 0.5569(3) 0.7046(7) 0.037(2) Uani 1 1 d .
H2 H 0.5675 0.5612 0.7714 0.044 Uiso 1 1 calc R
N3 N 0.5045(2) 0.6064(2) 0.7084(6) 0.042(2) Uani 1 1 d .
H3A H 0.5083 0.6104 0.7709 0.050 Uiso 1 1 calc R
H3B H 0.4843 0.6201 0.6778 0.050 Uiso 1 1 calc R
C3 C 0.5296(3) 0.5790(3) 0.6591(6) 0.028(2) Uani 1 1 d .
N4 N 0.5183(2) 0.5917(3) 0.1816(6) 0.048(2) Uani 1 1 d .
H4A H 0.5165 0.5864 0.1191 0.057 Uiso 1 1 calc R
H4B H 0.5135 0.6174 0.2033 0.057 Uiso 1 1 calc R
C4 C 0.5245(3) 0.5729(3) 0.5589(6) 0.027(2) Uani 1 1 d .
H4 H 0.5040 0.5886 0.5240 0.033 Uiso 1 1 calc R
N5 N 0.6578(2) 0.5073(2) 0.3955(5) 0.0281(18) Uani 1 1 d .
C5 C 0.5493(3) 0.5441(3) 0.5118(6) 0.027(2) Uani 1 1 d .
N6 N 0.6724(2) 0.4502(2) 0.5408(5) 0.0263(17) Uani 1 1 d .
C6 C 0.5449(2) 0.5365(3) 0.4056(6) 0.026(2) Uani 1 1 d .
N7 N 0.7415(3) 0.6070(2) 0.3556(5) 0.043(2) Uani 1 1 d .
H7A H 0.7662 0.6072 0.3845 0.051 Uiso 1 1 calc R
H7B H 0.7339 0.6283 0.3188 0.051 Uiso 1 1 calc R
C7 C 0.5321(3) 0.5684(3) 0.3436(6) 0.032(2) Uani 1 1 d .
H7 H 0.5260 0.5956 0.3687 0.038 Uiso 1 1 calc R
N8 N 0.7936(2) 0.4032(3) 0.5814(5) 0.040(2) Uani 1 1 d .
H8A H 0.8154 0.4150 0.5526 0.048 Uiso 1 1 calc R
H8B H 0.7973 0.3807 0.6180 0.048 Uiso 1 1 calc R
C8 C 0.5282(3) 0.5607(3) 0.2438(7) 0.035(2) Uani 1 1 d .
N9 N 0.5772(2) 0.4120(2) 0.5685(5) 0.0290(18) Uani 1 1 d .
C9 C 0.5360(3) 0.5199(3) 0.2120(6) 0.034(2) Uani 1 1 d .
H9 H 0.5320 0.5128 0.1457 0.040 Uiso 1 1 calc R
N10 N 0.6066(2) 0.4011(2) 0.3832(5) 0.0315(18) Uani 1 1 d .
C10 C 0.5494(3) 0.4901(3) 0.2766(7) 0.039(2) Uani 1 1 d .
H10 H 0.5551 0.4626 0.2529 0.046 Uiso 1 1 calc R
N11 N 0.5774(3) 0.3084(3) 0.7561(6) 0.067(3) Uani 1 1 d .
H11A H 0.5810 0.2828 0.7332 0.081 Uiso 1 1 calc R
H11B H 0.5744 0.3124 0.8188 0.081 Uiso 1 1 calc R
C11 C 0.6488(3) 0.5403(3) 0.3394(6) 0.032(2) Uani 1 1 d .
H11 H 0.6220 0.5408 0.3086 0.038 Uiso 1 1 calc R
N12 N 0.5731(3) 0.2927(2) 0.2312(6) 0.045(2) Uani 1 1 d .
H12A H 0.5604 0.2720 0.2621 0.054 Uiso 1 1 calc R
H12B H 0.5780 0.2906 0.1686 0.054 Uiso 1 1 calc R
C12 C 0.6752(3) 0.5732(3) 0.3233(6) 0.032(2) Uani 1 1 d .
H12 H 0.6668 0.5957 0.2822 0.039 Uiso 1 1 calc R
C13 C 0.7152(3) 0.5738(3) 0.3677(7) 0.034(2) Uani 1 1 d .
C14 C 0.7248(3) 0.5388(3) 0.4247(6) 0.030(2) Uani 1 1 d .
H14 H 0.7516 0.5372 0.4554 0.036 Uiso 1 1 calc R
C15 C 0.6964(3) 0.5065(3) 0.4374(6) 0.024(2) Uiso 1 1 d .
C16 C 0.7061(3) 0.4698(3) 0.4985(6) 0.023(2) Uani 1 1 d .
C17 C 0.7465(3) 0.4552(3) 0.5119(6) 0.024(2) Uani 1 1 d .
H17 H 0.7695 0.4694 0.4819 0.029 Uiso 1 1 calc R
C18 C 0.7543(3) 0.4196(3) 0.5692(6) 0.029(2) Uani 1 1 d .
C19 C 0.7193(3) 0.4005(3) 0.6134(6) 0.027(2) Uani 1 1 d .
H19 H 0.7227 0.3767 0.6546 0.032 Uiso 1 1 calc R
C20 C 0.6803(3) 0.4169(3) 0.5956(6) 0.027(2) Uiso 1 1 d .
H20 H 0.6569 0.4032 0.6251 0.032 Uiso 1 1 calc R
C21 C 0.5721(3) 0.4157(3) 0.6646(7) 0.035(2) Uani 1 1 d .
H21 H 0.5687 0.4434 0.6898 0.042 Uiso 1 1 calc R
C22 C 0.5713(3) 0.3835(3) 0.7285(7) 0.040(3) Uani 1 1 d .
H22 H 0.5674 0.3887 0.7958 0.049 Uiso 1 1 calc R
C23 C 0.5764(3) 0.3422(3) 0.6938(7) 0.045(3) Uani 1 1 d .
C24 C 0.5810(3) 0.3372(3) 0.5937(7) 0.037(2) Uani 1 1 d .
H24 H 0.5839 0.3098 0.5666 0.045 Uiso 1 1 calc R
C25 C 0.5815(2) 0.3723(3) 0.5339(6) 0.027(2) Uani 1 1 d .
C26 C 0.5890(2) 0.3680(3) 0.4277(6) 0.026(2) Uani 1 1 d .
C27 C 0.5773(3) 0.3315(3) 0.3795(6) 0.030(2) Uani 1 1 d .
H27 H 0.5642 0.3092 0.4141 0.035 Uiso 1 1 calc R
C28 C 0.5849(3) 0.3275(3) 0.2795(7) 0.031(2) Uani 1 1 d .
C29 C 0.6056(3) 0.3616(3) 0.2343(7) 0.037(2) Uani 1 1 d .
H29 H 0.6123 0.3608 0.1672 0.044 Uiso 1 1 calc R
C30 C 0.61542(13) 0.39446(13) 0.2878(3) 0.038(2) Uani 1 1 d .
H30 H 0.6305 0.4163 0.2559 0.045 Uiso 1 1 calc R
Cl3 Cl 0.70969(13) 0.68342(13) 0.2161(3) 0.1039(17) Uani 0.75 1 d PR
Cl2 Cl 0.55771(13) 0.29932(13) -0.0023(3) 0.107(3) Uani 0.50 1 d PR
Cl1 Cl 0.50000(13) 0.25000(13) 0.3750(3) 0.0472(14) Uani 1 4 d SR
O3 O 0.4816(2) 0.6074(3) 0.9350(5) 0.079(3) Uani 1 1 d .
O2 O 0.8845(2) 0.4198(2) 0.5899(7) 0.076(3) Uani 1 1 d .
Cl4 Cl 0.5432(4) 0.5524(3) -0.0400(5) 0.144(4) Uani 0.50 1 d P
O4 O 0.5000 0.2500 -0.1250 0.138(8) Uani 1 4 d S
O1 O 0.5980(5) 0.3639(5) -0.0331(11) 0.062(4) Uiso 0.50 1 d P
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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
N1 Cd1 N10 158.5(2)
N1 Cd1 N9 95.9(3)
N10 Cd1 N9 71.9(2)
N1 Cd1 N2 72.0(2)
N10 Cd1 N2 95.8(3)
N9 Cd1 N2 112.0(2)
N1 Cd1 N5 91.8(2)
N10 Cd1 N5 105.8(2)
N9 Cd1 N5 159.3(2)
N2 Cd1 N5 88.7(2)
N1 Cd1 N6 105.0(2)
N10 Cd1 N6 92.5(2)
N9 Cd1 N6 88.4(2)
N2 Cd1 N6 159.5(2)
N5 Cd1 N6 71.0(2)
C1 N1 C5 116.2(8)
C1 N1 Cd1 126.4(6)
C5 N1 Cd1 116.3(5)
N1 C1 C2 124.7(8)
C6 N2 C10 116.6(8)
C6 N2 Cd1 112.9(5)
C10 N2 Cd1 124.3(6)
C1 C2 C3 118.7(8)
N3 C3 C2 121.8(8)
N3 C3 C4 120.9(8)
C2 C3 C4 117.3(8)
C5 C4 C3 119.6(8)
C11 N5 C15 117.1(7)
C11 N5 Cd1 123.7(6)
C15 N5 Cd1 115.5(5)
N1 C5 C4 123.4(8)
N1 C5 C6 115.3(8)
C4 C5 C6 121.3(8)
C20 N6 C16 117.4(7)
C20 N6 Cd1 124.0(6)
C16 N6 Cd1 115.4(5)
N2 C6 C7 122.3(8)
N2 C6 C5 116.6(8)
C7 C6 C5 121.1(8)
C6 C7 C8 120.3(9)
N4 C8 C9 121.4(9)
N4 C8 C7 121.3(9)
C9 C8 C7 117.2(9)
C21 N9 C25 116.3(8)
C21 N9 Cd1 124.1(6)
C25 N9 Cd1 114.5(5)
C10 C9 C8 119.5(9)
C26 N10 C30 114.1(6)
C26 N10 Cd1 116.0(6)
C30 N10 Cd1 128.8(5)
N2 C10 C9 123.9(9)
N5 C11 C12 124.6(9)
C11 C12 C13 119.6(8)
N7 C13 C14 123.7(9)
N7 C13 C12 120.8(9)
C14 C13 C12 115.5(8)
C15 C14 C13 121.5(8)
N5 C15 C14 121.6(8)
N5 C15 C16 116.6(7)
C14 C15 C16 121.8(8)
N6 C16 C17 121.1(8)
N6 C16 C15 116.3(7)
C17 C16 C15 122.6(8)
C16 C17 C18 120.7(8)
N8 C18 C17 122.6(8)
N8 C18 C19 120.3(8)
C17 C18 C19 117.1(8)
C20 C19 C18 118.3(8)
N6 C20 C19 125.4(8)
N9 C21 C22 125.5(9)
C21 C22 C23 118.8(9)
N11 C23 C24 121.8(10)
N11 C23 C22 121.2(9)
C24 C23 C22 117.0(9)
C25 C24 C23 119.8(9)
N9 C25 C24 122.5(8)
N9 C25 C26 116.6(8)
C24 C25 C26 120.8(8)
N10 C26 C27 123.1(8)
N10 C26 C25 116.5(8)
C27 C26 C25 120.4(8)
C26 C27 C28 120.2(8)
N12 C28 C27 121.1(8)
N12 C28 C29 122.7(9)
C27 C28 C29 116.2(8)
C30 C29 C28 118.1(8)
C29 C30 N10 128.1(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cd1 N1 2.321(7)
Cd1 N10 2.334(7)
Cd1 N9 2.340(7)
Cd1 N2 2.349(7)
Cd1 N5 2.360(7)
Cd1 N6 2.360(7)
N1 C1 1.334(11)
N1 C5 1.353(11)
C1 C2 1.381(13)
N2 C6 1.351(11)
N2 C10 1.367(11)
C2 C3 1.386(12)
N3 C3 1.361(11)
C3 C4 1.405(12)
N4 C8 1.344(12)
C4 C5 1.369(12)
N5 C11 1.332(11)
N5 C15 1.355(10)
C5 C6 1.492(12)
N6 C20 1.323(10)
N6 C16 1.368(10)
C6 C7 1.385(12)
N7 C13 1.351(11)
C7 C8 1.402(13)
N8 C18 1.364(11)
C8 C9 1.388(13)
N9 C21 1.340(11)
N9 C25 1.352(11)
C9 C10 1.367(13)
N10 C26 1.338(11)
N10 C30 1.361(8)
N11 C23 1.372(13)
C11 C12 1.358(12)
N12 C28 1.341(11)
C12 C13 1.409(13)
C13 C14 1.396(13)
C14 C15 1.374(12)
C15 C16 1.468(12)
C16 C17 1.376(12)
C17 C18 1.400(12)
C18 C19 1.403(12)
C19 C20 1.363(11)
C21 C22 1.350(13)
C22 C23 1.406(14)
C23 C24 1.398(13)
C24 C25 1.387(12)
C25 C26 1.490(12)
C26 C27 1.386(12)
C27 C28 1.405(12)
C28 C29 1.412(13)
C29 C30 1.314(10)
