#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:07:06 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179913 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/08/7020827.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_7020827
loop_
_publ_author_name
'Dey, Rajdip'
'Bhattacharya, Biswajit'
'Colacio, Enrique'
'Ghoshal, Debajyoti'
_publ_section_title
;
 Fabrication of metal-organic hybrid architectures using bridging diphenyl
 phosphate: Syntheses, characterization, magnetic properties and the
 effect of weak interactions on their crystal packing.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2094
_journal_page_last               2106
_journal_paper_doi               10.1039/c2dt32057f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C50 H50 N4 Ni O9 P2'
_chemical_formula_weight         971.59
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 109.5670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7300(4)
_cell_length_b                   18.3498(4)
_cell_length_c                   19.7497(5)
_cell_measurement_reflns_used    39944
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      1.9
_cell_volume                     4688.4(2)
_computing_cell_refinement       'SMART APEX II'
_computing_data_collection       'SMART APEX II (Bruker,2010)'
_computing_data_reduction        'SAINT (Bruker,2000)'
_computing_molecular_graphics    'Ortep-3v2 for windows (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39944
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  0.8892
_exptl_absorpt_correction_T_min  0.8281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'XPREP' - A PROGRAM DATA PREPARATION & RECIPROCAL
SPACE EXPLORATION,
Bruker Analytical X-ray Systems, 1997
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5780
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0322
_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)+(0.0451P)²+2.5421P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0899
_reflns_number_gt                4681
_reflns_number_total             5780
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c2dt32057f.txt
_cod_data_source_block           complex6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7020827
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
C1 C 0.88970(12) -0.07243(9) 0.34976(8) 0.0361(3) Uani 1 1 d .
H1 H 0.9550 -0.0912 0.3558 0.043 Uiso 1 1 calc R
C2 C 0.81026(12) -0.08926(9) 0.28741(8) 0.0383(4) Uani 1 1 d .
H2 H 0.8229 -0.1190 0.2531 0.046 Uiso 1 1 calc R
C3 C 0.71207(12) -0.06230(8) 0.27556(8) 0.0328(3) Uani 1 1 d .
C4 C 0.70029(14) -0.01844(12) 0.32891(10) 0.0520(5) Uani 1 1 d .
H4 H 0.6360 0.0017 0.3237 0.062 Uiso 1 1 calc R
C5 C 0.78341(14) -0.00431(11) 0.38993(10) 0.0520(5) Uani 1 1 d .
H5 H 0.7727 0.0255 0.4249 0.062 Uiso 1 1 calc R
C6 C 0.62407(12) -0.07776(9) 0.20723(9) 0.0385(4) Uani 1 1 d .
H6A H 0.6328 -0.0482 0.1690 0.046 Uiso 1 1 calc R
H6B H 0.5599 -0.0631 0.2137 0.046 Uiso 1 1 calc R
C7 C 0.61542(13) -0.15701(9) 0.18425(10) 0.0445(4) Uani 1 1 d .
H7A H 0.6169 -0.1874 0.2248 0.053 Uiso 1 1 calc R
H7B H 0.6748 -0.1697 0.1705 0.053 Uiso 1 1 calc R
C8 C 0.51723(13) -0.17311(9) 0.12174(10) 0.0442(4) Uani 1 1 d .
H8A H 0.4579 -0.1658 0.1372 0.053 Uiso 1 1 calc R
H8B H 0.5118 -0.1391 0.0831 0.053 Uiso 1 1 calc R
C9 C 0.51521(11) -0.24983(9) 0.09398(9) 0.0360(3) Uani 1 1 d .
C10 C 0.50719(14) -0.31039(10) 0.13381(9) 0.0438(4) Uani 1 1 d .
H10 H 0.5029 -0.3043 0.1795 0.053 Uiso 1 1 calc R
C11 C 0.50552(13) -0.37936(9) 0.10624(9) 0.0390(4) Uani 1 1 d .
H11 H 0.4999 -0.4188 0.1343 0.047 Uiso 1 1 calc R
C12 C 0.52104(13) -0.33436(9) 0.00317(8) 0.0371(3) Uani 1 1 d .
H12 H 0.5267 -0.3419 -0.0419 0.045 Uiso 1 1 calc R
C13 C 0.52294(13) -0.26354(9) 0.02710(9) 0.0388(3) Uani 1 1 d .
H13 H 0.5294 -0.2250 -0.0017 0.047 Uiso 1 1 calc R
C14 C 0.66013(12) 0.09356(9) 0.48624(9) 0.0369(3) Uani 1 1 d .
C15 C 0.56405(14) 0.06946(10) 0.44353(10) 0.0478(4) Uani 1 1 d .
H15 H 0.5350 0.0283 0.4565 0.057 Uiso 1 1 calc R
C16 C 0.51132(16) 0.10683(12) 0.38136(11) 0.0605(5) Uani 1 1 d .
H16 H 0.4463 0.0910 0.3526 0.073 Uiso 1 1 calc R
C17 C 0.55457(18) 0.16720(12) 0.36188(11) 0.0630(6) Uani 1 1 d .
H17 H 0.5191 0.1921 0.3198 0.076 Uiso 1 1 calc R
C18 C 0.65035(17) 0.19078(11) 0.40463(11) 0.0572(5) Uani 1 1 d .
H18 H 0.6796 0.2316 0.3911 0.069 Uiso 1 1 calc R
C19 C 0.70397(14) 0.15454(10) 0.46769(10) 0.0452(4) Uani 1 1 d .
H19 H 0.7683 0.1711 0.4969 0.054 Uiso 1 1 calc R
C20 C 0.78742(13) -0.07718(10) 0.64010(10) 0.0436(4) Uani 1 1 d .
C21 C 0.78526(16) -0.11251(12) 0.70130(13) 0.0623(6) Uani 1 1 d .
H21 H 0.8080 -0.0892 0.7456 0.075 Uiso 1 1 calc R
C22 C 0.7487(2) -0.18322(15) 0.69545(19) 0.0906(9) Uani 1 1 d .
H22 H 0.7465 -0.2075 0.7362 0.109 Uiso 1 1 calc R
C23 C 0.7158(2) -0.21788(14) 0.6302(2) 0.0960(10) Uani 1 1 d .
H23 H 0.6922 -0.2657 0.6268 0.115 Uiso 1 1 calc R
C24 C 0.71784(18) -0.18180(13) 0.57007(17) 0.0764(7) Uani 1 1 d .
H24 H 0.6947 -0.2053 0.5258 0.092 Uiso 1 1 calc R
C25 C 0.75382(15) -0.11068(11) 0.57412(12) 0.0556(5) Uani 1 1 d .
H25 H 0.7551 -0.0863 0.5331 0.067 Uiso 1 1 calc R
N1 N 0.87815(10) -0.03068(7) 0.40201(7) 0.0329(3) Uani 1 1 d .
N2 N 0.51157(9) -0.39260(7) 0.04094(7) 0.0315(3) Uani 1 1 d .
O1W O 1.0000 0.19526(14) 0.7500 0.0807(8) Uani 1 2 d S
O5 O 0.88576(8) 0.02338(6) 0.54598(6) 0.0353(2) Uani 1 1 d .
O6 O 0.70714(9) 0.05356(7) 0.54810(6) 0.0423(3) Uani 1 1 d .
O7 O 0.86323(10) 0.12117(6) 0.63073(6) 0.0448(3) Uani 1 1 d .
O8 O 0.82649(10) -0.00681(6) 0.65142(6) 0.0427(3) Uani 1 1 d .
P2 P 0.82926(3) 0.05203(2) 0.59243(2) 0.03146(10) Uani 1 1 d .
Ni1 Ni 1.0000 0.0000 0.5000 0.02686(8) Uani 1 2 d S
H1W H 0.963(2) 0.1687(15) 0.7162(14) 0.096(10) Uiso 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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
N1 C1 C2 123.71(14) . .
C1 C2 C3 120.43(14) . .
C4 C3 C2 115.97(14) . .
C4 C3 C6 122.06(14) . .
C2 C3 C6 121.94(14) . .
C3 C4 C5 120.22(16) . .
N1 C5 C4 124.13(16) . .
C3 C6 C7 114.06(14) . .
C6 C7 C8 112.86(14) . .
C9 C8 C7 112.33(14) . .
C13 C9 C10 116.24(15) . .
C13 C9 C8 121.27(16) . .
C10 C9 C8 122.49(15) . .
C11 C10 C9 120.45(15) . .
N2 C11 C10 123.30(15) . .
N2 C12 C13 123.84(15) . .
C12 C13 C9 119.97(15) . .
C19 C14 C15 120.77(16) . .
C19 C14 O6 123.30(15) . .
C15 C14 O6 115.92(15) . .
C14 C15 C16 119.60(18) . .
C17 C16 C15 120.2(2) . .
C16 C17 C18 119.83(19) . .
C17 C18 C19 120.82(19) . .
C14 C19 C18 118.75(18) . .
C25 C20 C21 121.44(19) . .
C25 C20 O8 123.95(17) . .
C21 C20 O8 114.61(18) . .
C20 C21 C22 118.8(3) . .
C23 C22 C21 120.7(3) . .
C24 C23 C22 119.7(2) . .
C23 C24 C25 121.0(3) . .
C20 C25 C24 118.4(2) . .
C5 N1 C1 115.53(13) . .
C5 N1 Ni1 118.76(10) . .
C1 N1 Ni1 125.66(10) . .
C12 N2 C11 116.18(13) . .
C12 N2 Ni1 122.77(10) . 4_645
C11 N2 Ni1 121.00(10) . 4_645
P2 O5 Ni1 163.81(7) . .
C14 O6 P2 125.52(10) . .
C20 O8 P2 127.84(12) . .
O7 P2 O5 118.87(7) . .
O7 P2 O8 106.78(7) . .
O5 P2 O8 110.91(7) . .
O7 P2 O6 110.95(7) . .
O5 P2 O6 109.58(6) . .
O8 P2 O6 97.67(6) . .
O5 Ni1 O5 180.00(4) . 5_756
O5 Ni1 N2 90.21(5) . 4_655
O5 Ni1 N2 89.79(5) 5_756 4_655
O5 Ni1 N2 89.79(5) . 8_546
O5 Ni1 N2 90.21(5) 5_756 8_546
N2 Ni1 N2 180.000(1) 4_655 8_546
O5 Ni1 N1 88.53(4) . .
O5 Ni1 N1 91.47(4) 5_756 .
N2 Ni1 N1 87.93(5) 4_655 .
N2 Ni1 N1 92.07(5) 8_546 .
O5 Ni1 N1 91.47(4) . 5_756
O5 Ni1 N1 88.53(4) 5_756 5_756
N2 Ni1 N1 92.07(5) 4_655 5_756
N2 Ni1 N1 87.93(5) 8_546 5_756
N1 Ni1 N1 180.00(5) . 5_756
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.3366(19) .
C1 C2 1.379(2) .
C2 C3 1.381(2) .
C3 C4 1.378(2) .
C3 C6 1.507(2) .
C4 C5 1.379(2) .
C5 N1 1.332(2) .
C6 C7 1.516(2) .
C7 C8 1.521(2) .
C8 C9 1.508(2) .
C9 C13 1.383(2) .
C9 C10 1.387(2) .
C10 C11 1.375(2) .
C11 N2 1.342(2) .
C12 N2 1.334(2) .
C12 C13 1.380(2) .
C14 C19 1.377(2) .
C14 C15 1.379(2) .
C14 O6 1.3855(19) .
C15 C16 1.381(3) .
C16 C17 1.371(3) .
C17 C18 1.373(3) .
C18 C19 1.386(3) .
C20 C25 1.373(3) .
C20 C21 1.381(3) .
C20 O8 1.388(2) .
C21 C22 1.382(3) .
C22 C23 1.371(4) .
C23 C24 1.368(4) .
C24 C25 1.388(3) .
N1 Ni1 2.1662(12) .
N2 Ni1 2.1158(12) 4_645
O5 P2 1.4820(11) .
O5 Ni1 2.1030(10) .
O6 P2 1.6111(12) .
O7 P2 1.4707(12) .
O8 P2 1.5982(12) .
Ni1 O5 2.1030(10) 5_756
Ni1 N2 2.1158(12) 4_655
Ni1 N2 2.1158(12) 8_546
Ni1 N1 2.1662(12) 5_756
