#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:46:15 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179595 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/59/4505941.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_4505941
loop_
_publ_author_name
'Carrión, M. Carmen'
'Durá, Gema'
'Jalón, Félix A.'
'Manzano, Blanca R.'
'Rodríguez, Ana M.'
_publ_section_title
;
 Polynuclear Complexes Containing Ditopic Bispyrazolylmethane Ligands.
 Influence of Metal Geometry and Supramolecular Interactions
;
_journal_issue                   4
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1952
_journal_paper_doi               10.1021/cg201677s
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C38 H52 N14 Ni2 O8, 3(C3 H7 N O), 2(N O3)'
_chemical_formula_sum            'C47 H73 N19 Ni2 O17'
_chemical_formula_weight         1293.62
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                115.960(4)
_cell_angle_beta                 95.722(5)
_cell_angle_gamma                103.508(5)
_cell_formula_units_Z            1
_cell_length_a                   10.1334(12)
_cell_length_b                   13.8385(6)
_cell_length_c                   13.9286(6)
_cell_measurement_reflns_used    982
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      25.426
_cell_measurement_theta_min      2.215
_cell_volume                     1661.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega and phi 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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16858
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_T_max  0.9270
_exptl_absorpt_correction_T_min  0.8879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.420
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1449P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2109
_refine_ls_wR_factor_ref         0.2351
_reflns_number_gt                5896
_reflns_number_total             7912
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201677s_si_002.cif
_cod_data_source_block           10
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4505941
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Ni1 Ni 0.76653(4) 0.12096(4) 0.75564(3) 0.02917(18) Uani 1 1 d .
O1 O 0.9659(3) 0.1896(2) 0.7330(2) 0.0417(6) Uani 1 1 d .
O2 O 0.9099(3) 0.0252(2) 0.7235(2) 0.0393(6) Uani 1 1 d .
O3 O 1.1137(3) 0.0939(3) 0.7040(3) 0.0634(9) Uani 1 1 d .
O4 O 0.8702(3) 0.1864(3) 0.9149(2) 0.0458(7) Uani 1 1 d .
N1 N 0.6757(3) 0.2465(3) 0.7921(3) 0.0342(7) Uani 1 1 d .
N2 N 0.5414(3) 0.2337(2) 0.8073(2) 0.0290(6) Uani 1 1 d .
N3 N 0.6015(3) 0.0207(3) 0.7798(2) 0.0301(6) Uani 1 1 d .
N4 N 0.4880(3) 0.0541(2) 0.8056(2) 0.0279(6) Uani 1 1 d .
N5 N 0.6989(3) 0.0464(3) 0.5865(2) 0.0286(6) Uani 1 1 d .
N6 N 1.0005(3) 0.1025(3) 0.7200(3) 0.0410(8) Uani 1 1 d .
N7 N 0.9009(4) 0.2586(3) 1.0967(3) 0.0455(8) Uani 1 1 d .
C1 C 0.5126(4) 0.3342(3) 0.8461(3) 0.0364(8) Uani 1 1 d .
C2 C 0.6312(5) 0.4123(3) 0.8574(4) 0.0456(10) Uani 1 1 d .
H2 H 0.6439 0.4888 0.8818 0.055 Uiso 1 1 calc R
C3 C 0.7314(5) 0.3566(3) 0.8255(4) 0.0432(9) Uani 1 1 d .
C4 C 0.3757(5) 0.3452(4) 0.8683(4) 0.0480(10) Uani 1 1 d .
H4A H 0.3753 0.4211 0.8891 0.072 Uiso 1 1 calc R
H4B H 0.3592 0.3283 0.9268 0.072 Uiso 1 1 calc R
H4C H 0.3036 0.2933 0.8033 0.072 Uiso 1 1 calc R
C5 C 0.8775(6) 0.4049(4) 0.8248(5) 0.0708(16) Uani 1 1 d .
H5A H 0.9349 0.3680 0.8458 0.106 Uiso 1 1 calc R
H5B H 0.9097 0.4843 0.8756 0.106 Uiso 1 1 calc R
H5C H 0.8826 0.3936 0.7523 0.106 Uiso 1 1 calc R
C6 C 0.4131(4) -0.0045(3) 0.8503(3) 0.0347(8) Uani 1 1 d .
C7 C 0.4844(4) -0.0755(4) 0.8557(3) 0.0400(9) Uani 1 1 d .
H7 H 0.4602 -0.1260 0.8829 0.048 Uiso 1 1 calc R
C8 C 0.6014(4) -0.0570(3) 0.8119(3) 0.0346(8) Uani 1 1 d .
C9 C 0.2814(4) 0.0125(4) 0.8841(4) 0.0452(10) Uani 1 1 d .
H9A H 0.2989 0.0904 0.9365 0.068 Uiso 1 1 calc R
H9B H 0.2491 -0.0343 0.9167 0.068 Uiso 1 1 calc R
H9C H 0.2117 -0.0077 0.8209 0.068 Uiso 1 1 calc R
C10 C 0.7117(5) -0.1130(4) 0.8004(4) 0.0508(11) Uani 1 1 d .
H10A H 0.7068 -0.1588 0.7240 0.076 Uiso 1 1 calc R
H10B H 0.6980 -0.1597 0.8354 0.076 Uiso 1 1 calc R
H10C H 0.8016 -0.0565 0.8345 0.076 Uiso 1 1 calc R
C11 C 0.4396(4) 0.1231(3) 0.7652(3) 0.0287(7) Uani 1 1 d .
H11 H 0.3572 0.1357 0.7938 0.034 Uiso 1 1 calc R
C12 C 0.6423(4) -0.0654(3) 0.5291(3) 0.0338(8) Uani 1 1 d .
H12 H 0.6337 -0.1070 0.5667 0.041 Uiso 1 1 calc R
C13 C 0.5962(4) -0.1219(3) 0.4177(3) 0.0338(8) Uani 1 1 d .
H13 H 0.5571 -0.2001 0.3812 0.041 Uiso 1 1 calc R
C14 C 0.6077(3) -0.0623(3) 0.3589(3) 0.0266(7) Uani 1 1 d .
C15 C 0.6688(4) 0.0535(3) 0.4173(3) 0.0328(8) Uani 1 1 d .
H15 H 0.6798 0.0967 0.3812 0.039 Uiso 1 1 calc R
C16 C 0.7133(4) 0.1042(3) 0.5300(3) 0.0338(8) Uani 1 1 d .
H16 H 0.7553 0.1821 0.5686 0.041 Uiso 1 1 calc R
C17 C 0.8310(4) 0.2332(3) 0.9998(3) 0.0388(9) Uani 1 1 d .
H17 H 0.7486 0.2513 0.9950 0.047 Uiso 1 1 calc R
C18 C 0.8548(6) 0.3175(5) 1.1968(4) 0.0666(15) Uani 1 1 d .
H18A H 0.7733 0.3358 1.1790 0.100 Uiso 1 1 calc R
H18B H 0.9278 0.3857 1.2473 0.100 Uiso 1 1 calc R
H18C H 0.8330 0.2695 1.2300 0.100 Uiso 1 1 calc R
C19 C 1.0285(6) 0.2277(6) 1.1064(5) 0.0806(19) Uani 1 1 d .
H19A H 1.0238 0.1623 1.0396 0.121 Uiso 1 1 calc R
H19B H 1.0375 0.2111 1.1664 0.121 Uiso 1 1 calc R
H19C H 1.1078 0.2895 1.1196 0.121 Uiso 1 1 calc R
N8 N 0.3665(5) 0.5489(4) 1.4629(4) 0.0637(11) Uani 1 1 d .
O5 O 0.5543(8) 0.6905(5) 1.4880(6) 0.151(3) Uani 1 1 d .
C21 C 0.4627(10) 0.5965(6) 1.4278(7) 0.104(3) Uani 1 1 d .
H21 H 0.4636 0.5587 1.3539 0.124 Uiso 1 1 calc R
C22 C 0.3628(9) 0.6072(7) 1.5768(6) 0.107(3) Uani 1 1 d .
H22A H 0.4534 0.6596 1.6189 0.161 Uiso 1 1 calc R
H22B H 0.3368 0.5533 1.6029 0.161 Uiso 1 1 calc R
H22C H 0.2958 0.6475 1.5846 0.161 Uiso 1 1 calc R
C23 C 0.2754(8) 0.4364(7) 1.3923(7) 0.114(3) Uani 1 1 d .
H23A H 0.2696 0.4197 1.3172 0.171 Uiso 1 1 calc R
H23B H 0.1843 0.4303 1.4072 0.171 Uiso 1 1 calc R
H23C H 0.3115 0.3837 1.4051 0.171 Uiso 1 1 calc R
N9 N 0.9356(5) 0.7006(4) 1.4618(4) 0.0214(10) Uani 0.50 1 d P
O6 O 1.1026(12) 0.7150(14) 1.5820(11) 0.139(5) Uani 0.50 1 d P
C24 C 1.0230(10) 0.6535(10) 1.4857(9) 0.059(3) Uani 0.50 1 d P
H24 H 1.0268 0.5824 1.4374 0.071 Uiso 0.50 1 calc PR
C25 C 0.9313(10) 0.8075(8) 1.5217(9) 0.061(3) Uani 0.50 1 d P
H25A H 0.9772 0.8366 1.5969 0.091 Uiso 0.50 1 calc PR
H25B H 0.8359 0.8068 1.5172 0.091 Uiso 0.50 1 calc PR
H25C H 0.9777 0.8545 1.4933 0.091 Uiso 0.50 1 calc PR
C26 C 0.8371(9) 0.6347(8) 1.3552(7) 0.048(2) Uani 0.50 1 d P
H26A H 0.8632 0.6661 1.3080 0.072 Uiso 0.50 1 calc PR
H26B H 0.7450 0.6367 1.3645 0.072 Uiso 0.50 1 calc PR
H26C H 0.8383 0.5578 1.3230 0.072 Uiso 0.50 1 calc PR
N10 N 0.4842(4) 0.3348(3) 1.1159(3) 0.0464(9) Uani 1 1 d .
O7 O 0.3603(4) 0.3240(3) 1.1130(4) 0.0770(12) Uani 1 1 d .
O8 O 0.5208(4) 0.2614(3) 1.0435(3) 0.0657(10) Uani 1 1 d .
O9 O 0.5718(6) 0.4194(4) 1.1880(4) 0.1118(18) 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'
Ni Ni 0.3393 1.1124 '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_3
O4 Ni1 N1 93.22(12) .
O4 Ni1 N3 90.34(12) .
N1 Ni1 N3 92.04(12) .
O4 Ni1 N5 168.07(11) .
N1 Ni1 N5 96.26(11) .
N3 Ni1 N5 96.54(12) .
O4 Ni1 O2 82.90(11) .
N1 Ni1 O2 164.52(12) .
N3 Ni1 O2 102.93(11) .
N5 Ni1 O2 86.05(10) .
O4 Ni1 O1 84.60(12) .
N1 Ni1 O1 104.40(12) .
N3 Ni1 O1 163.01(11) .
N5 Ni1 O1 86.03(11) .
O2 Ni1 O1 60.39(11) .
N6 O1 Ni1 91.4(2) .
N6 O2 Ni1 91.9(2) .
C17 O4 Ni1 129.0(3) .
C3 N1 N2 105.3(3) .
C3 N1 Ni1 130.7(3) .
N2 N1 Ni1 122.9(2) .
C1 N2 N1 111.3(3) .
C1 N2 C11 125.6(3) .
N1 N2 C11 121.9(3) .
C8 N3 N4 105.8(3) .
C8 N3 Ni1 128.8(2) .
N4 N3 Ni1 121.3(2) .
C6 N4 N3 111.6(3) .
C6 N4 C11 125.4(3) .
N3 N4 C11 121.4(3) .
C12 N5 C16 117.3(3) .
C12 N5 Ni1 119.1(2) .
C16 N5 Ni1 123.6(3) .
O3 N6 O2 121.8(4) .
O3 N6 O1 122.0(4) .
O2 N6 O1 116.2(3) .
C17 N7 C19 119.9(4) .
C17 N7 C18 121.7(4) .
C19 N7 C18 118.3(4) .
C2 C1 N2 105.9(3) .
C2 C1 C4 131.0(4) .
N2 C1 C4 123.1(4) .
C1 C2 C3 107.6(4) .
N1 C3 C2 109.8(4) .
N1 C3 C5 121.7(4) .
C2 C3 C5 128.5(4) .
N4 C6 C7 105.9(3) .
N4 C6 C9 123.5(3) .
C7 C6 C9 130.7(3) .
C6 C7 C8 106.7(3) .
N3 C8 C7 109.9(3) .
N3 C8 C10 122.6(3) .
C7 C8 C10 127.5(3) .
N2 C11 N4 112.0(3) .
N2 C11 C14 112.5(3) 2_656
N4 C11 C14 111.9(3) 2_656
N5 C12 C13 123.2(3) .
C12 C13 C14 119.9(3) .
C15 C14 C13 117.5(3) .
C15 C14 C11 121.4(3) 2_656
C13 C14 C11 121.0(3) 2_656
C14 C15 C16 119.0(3) .
N5 C16 C15 123.1(3) .
O4 C17 N7 122.7(4) .
C21 N8 C22 118.6(6) .
C21 N8 C23 120.4(6) .
C22 N8 C23 120.6(6) .
O5 C21 N8 123.8(8) .
C24 N9 C25 127.7(8) .
C24 N9 C26 117.1(8) .
C25 N9 C26 115.1(7) .
O6 C24 N9 113.3(11) .
O9 N10 O7 119.9(5) .
O9 N10 O8 119.8(5) .
O7 N10 O8 120.3(4) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O4 2.044(3) .
Ni1 N1 2.048(3) .
Ni1 N3 2.067(3) .
Ni1 N5 2.074(3) .
Ni1 O2 2.139(3) .
Ni1 O1 2.139(3) .
O1 N6 1.276(4) .
O2 N6 1.258(4) .
O3 N6 1.212(4) .
O4 C17 1.232(5) .
N1 C3 1.335(5) .
N1 N2 1.380(4) .
N2 C1 1.369(4) .
N2 C11 1.452(5) .
N3 C8 1.334(4) .
N3 N4 1.361(4) .
N4 C6 1.367(4) .
N4 C11 1.449(4) .
N5 C12 1.332(5) .
N5 C16 1.342(4) .
N7 C17 1.314(5) .
N7 C19 1.465(6) .
N7 C18 1.463(6) .
C1 C2 1.358(6) .
C1 C4 1.479(6) .
C2 C3 1.406(6) .
C3 C5 1.478(7) .
C6 C7 1.371(5) .
C6 C9 1.494(5) .
C7 C8 1.407(5) .
C8 C10 1.485(5) .
C11 C14 1.517(5) 2_656
C12 C13 1.363(5) .
C13 C14 1.388(4) .
C14 C15 1.382(5) .
C14 C11 1.517(5) 2_656
C15 C16 1.381(5) .
N8 C21 1.304(9) .
N8 C22 1.440(8) .
N8 C23 1.432(9) .
O5 C21 1.259(10) .
N9 C24 1.312(10) .
N9 C25 1.357(10) .
N9 C26 1.458(10) .
O6 C24 1.280(16) .
N10 O9 1.214(6) .
N10 O7 1.224(5) .
N10 O8 1.241(5) .
