#------------------------------------------------------------------------------
#$Date: 2019-10-24 03:55:08 +0300 (Thu, 24 Oct 2019) $
#$Revision: 219473 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/14/7701418.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_7701418
loop_
_publ_author_name
'Palion-Gazda, Joanna'
'Choroba, Katarzyna'
'Machura, Barbara'
'Świtlicka, Anna'
'Kruszyński, Rafał'
'Cano, Joan'
'Lloret, Francesc'
'Julve, Miguel'
_publ_section_title
;
 Influence of the pyrazine substituent on the structure and magnetic
 properties of dicyanamide-bridged cobalt(II) complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT02976A
_journal_year                    2019
_chemical_formula_moiety         'C32 H23 Co3 N28 O7'
_chemical_formula_sum            'C32 H23 Co3 N28 O7'
_chemical_formula_weight         1088.57
_chemical_name_systematic        '[Co3(dca)6(HOpyz)5(H2O)2]n'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-09-14 deposited with the CCDC.    2019-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                93.330(3)
_cell_angle_beta                 95.046(4)
_cell_angle_gamma                95.499(3)
_cell_formula_units_Z            1
_cell_length_a                   6.9942(3)
_cell_length_b                   12.0232(4)
_cell_length_c                   12.8819(6)
_cell_measurement_reflns_used    4608
_cell_measurement_temperature    295.0(2)
_cell_measurement_theta_max      28.8560
_cell_measurement_theta_min      3.7020
_cell_volume                     1071.69(8)
_computing_cell_refinement       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_molecular_graphics
'Mercury (Macrae, J.Appl.Cryst. 41 (2008) 466-470'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295.0(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Gemini A Ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7963
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         3.412
_exptl_absorpt_coefficient_mu    1.231
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. A51 (1995) 33-38'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.099
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         3781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0298P)²+0.4181P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3275
_reflns_number_total             3781
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02976a2.cif
_cod_data_source_block           co47a
_cod_original_cell_volume        1071.70(8)
_cod_database_code               7701418
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4714(3) 0.07822(18) 0.38759(18) 0.0281(5) Uani 1 1 d . . . . .
H1 H 0.4086 0.0277 0.3353 0.034 Uiso 1 1 calc R U . . .
C2 C 0.3588(4) 0.11946(18) 0.46706(17) 0.0275(5) Uani 1 1 d . . . . .
C3 C 0.6515(4) 0.2280(2) 0.53459(19) 0.0357(6) Uani 1 1 d . . . . .
H3 H 0.7158 0.2807 0.5845 0.043 Uiso 1 1 calc R U . . .
C4 C 0.7489(4) 0.18100(19) 0.46094(18) 0.0330(6) Uani 1 1 d . . . . .
H4 H 0.8814 0.1990 0.4623 0.040 Uiso 1 1 calc R U . . .
C5 C 1.0468(4) -0.0546(2) 0.08377(18) 0.0338(6) Uani 1 1 d . . . . .
C6 C 0.8722(4) 0.0721(2) 0.00854(19) 0.0389(6) Uani 1 1 d . . . . .
H6 H 0.7827 0.1243 0.0118 0.047 Uiso 1 1 calc R U . . .
C7 C -0.1025(4) 0.60920(18) 0.20895(18) 0.0305(5) Uani 1 1 d . . . . .
H7 H -0.0470 0.6730 0.1813 0.037 Uiso 1 1 calc R U . . .
C8 C -0.1698(4) 0.62191(19) 0.31050(19) 0.0327(6) Uani 1 1 d . . . . .
C9 C -0.2598(4) 0.4253(2) 0.2873(2) 0.0442(7) Uani 1 1 d . . . . .
H9 H -0.3149 0.3604 0.3134 0.053 Uiso 1 1 calc R U . . .
C10 C -0.1955(4) 0.42113(19) 0.1931(2) 0.0369(6) Uani 1 1 d . . . . .
H10 H -0.2068 0.3530 0.1540 0.044 Uiso 1 1 calc R U . . .
C94 C 1.1236(4) 0.2545(2) 0.29054(18) 0.0325(6) Uani 1 1 d . . . . .
C95 C 1.2688(4) 0.4142(2) 0.3735(2) 0.0491(7) Uani 1 1 d . . . . .
C96 C 0.5350(4) -0.1832(2) 0.20115(19) 0.0349(6) Uani 1 1 d . . . . .
C97 C 0.3481(4) -0.3371(2) 0.1217(2) 0.0375(6) Uani 1 1 d . . . . .
C98 C 0.4615(4) 0.17784(19) 0.11041(19) 0.0325(6) Uani 1 1 d . . . . .
C99 C 0.2362(4) 0.2920(2) 0.04861(19) 0.0349(6) Uani 1 1 d . . . . .
N1 N 0.6549(3) 0.10667(15) 0.38364(14) 0.0275(4) Uani 1 1 d . . . . .
N2 N 0.4597(3) 0.19871(16) 0.53606(16) 0.0319(5) Uani 1 1 d . . . . .
N3 N 0.9157(3) 0.01807(15) 0.09346(14) 0.0275(4) Uani 1 1 d . . . . .
N4 N -0.1134(3) 0.51485(14) 0.15253(15) 0.0270(4) Uani 1 1 d . . . . .
N5 N -0.2449(4) 0.52412(18) 0.34531(19) 0.0417(6) Uani 1 1 d . . . . .
N91 N 0.9989(3) 0.18601(16) 0.26709(16) 0.0354(5) Uani 1 1 d . . . . .
N92 N 1.2753(3) 0.32555(19) 0.3118(2) 0.0528(7) Uani 1 1 d . . . . .
N93 N 1.2816(5) 0.4936(3) 0.4278(2) 0.0876(11) Uani 1 1 d . . . . .
N94 N 0.6033(3) -0.09288(17) 0.21605(16) 0.0348(5) Uani 1 1 d . . . . .
N95 N 0.4674(4) -0.2877(2) 0.1976(2) 0.0667(8) Uani 1 1 d . . . . .
N96 N 0.2429(3) -0.39029(17) 0.06182(17) 0.0390(5) Uani 1 1 d . . . . .
N97 N 0.5820(3) 0.14364(17) 0.16114(16) 0.0360(5) Uani 1 1 d . . . . .
N98 N 0.3297(4) 0.2047(2) 0.0428(2) 0.0672(8) Uani 1 1 d . . . . .
N99 N 0.1411(3) 0.36329(17) 0.04267(16) 0.0376(5) Uani 1 1 d . . . . .
O1 O 0.1875(2) 0.08831(14) 0.47452(13) 0.0373(4) Uani 1 1 d . . . . .
O2 O 1.1016(6) -0.1174(3) 0.1618(3) 0.0543(16) Uani 0.515(6) 1 d . . P A -1
H2 H 1.0665 -0.0920 0.2166 0.081 Uiso 0.515(6) 1 calc R U P A -1
O3 O -0.1612(3) 0.71264(14) 0.36337(14) 0.0444(5) Uani 1 1 d . . . . .
O99 O 0.9760(2) -0.04441(13) 0.32554(12) 0.0335(4) Uani 1 1 d . . . . .
H99A H 0.9106 -0.1021 0.3484 0.050 Uiso 1 1 d R U . . .
H99B H 1.0386 -0.0053 0.3795 0.050 Uiso 1 1 d R U . . .
Co1 Co 0.78429(4) 0.05564(2) 0.23906(2) 0.02300(10) Uani 1 1 d . . . . .
Co2 Co 0.0000 0.5000 0.0000 0.02200(12) Uani 1 2 d S . P . .
H2N H 0.395(4) 0.228(2) 0.581(2) 0.049(9) Uiso 1 1 d . . . . .
H5N H -0.279(4) 0.525(2) 0.403(2) 0.039(8) 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'
Co Co 0.3494 0.9721 '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
N1 C1 C2 124.7(2) . .
N1 C1 H1 117.7 . .
C2 C1 H1 117.7 . .
O1 C2 N2 121.6(2) . .
O1 C2 C1 125.0(2) . .
N2 C2 C1 113.4(2) . .
C4 C3 N2 120.1(2) . .
C4 C3 H3 120.0 . .
N2 C3 H3 120.0 . .
C3 C4 N1 120.8(2) . .
C3 C4 H4 119.6 . .
N1 C4 H4 119.6 . .
N3 C5 O2 122.1(2) . .
N3 C5 C6 121.4(2) . 2_755
O2 C5 C6 116.4(2) . 2_755
N3 C6 C5 123.3(2) . 2_755
N3 C6 H6 118.4 . .
C5 C6 H6 118.4 2_755 .
N4 C7 C8 124.8(2) . .
N4 C7 H7 117.6 . .
C8 C7 H7 117.6 . .
O3 C8 N5 122.1(2) . .
O3 C8 C7 124.4(2) . .
N5 C8 C7 113.4(2) . .
C10 C9 N5 120.0(2) . .
C10 C9 H9 120.0 . .
N5 C9 H9 120.0 . .
C9 C10 N4 121.5(2) . .
C9 C10 H10 119.3 . .
N4 C10 H10 119.3 . .
N91 C94 N92 174.2(3) . .
N93 C95 N92 173.6(4) . .
N94 C96 N95 171.9(3) . .
N96 C97 N95 172.4(3) . .
N97 C98 N98 171.3(3) . .
N99 C99 N98 171.5(3) . .
C1 N1 C4 118.0(2) . .
C1 N1 Co1 117.63(15) . .
C4 N1 Co1 123.51(15) . .
C3 N2 C2 122.7(2) . .
C3 N2 H2N 122(2) . .
C2 N2 H2N 116(2) . .
C6 N3 C5 115.3(2) . .
C6 N3 Co1 120.51(16) . .
C5 N3 Co1 124.17(15) . .
C7 N4 C10 117.6(2) . .
C7 N4 Co2 123.08(15) . .
C10 N4 Co2 119.33(15) . .
C9 N5 C8 122.7(2) . .
C9 N5 H5N 119.1(19) . .
C8 N5 H5N 118.2(19) . .
C94 N91 Co1 174.0(2) . .
C94 N92 C95 120.2(2) . .
C96 N94 Co1 167.2(2) . .
C96 N95 C97 123.8(2) . .
C97 N96 Co2 159.4(2) . 1_545
C98 N97 Co1 170.2(2) . .
C98 N98 C99 126.8(2) . .
C99 N99 Co2 166.4(2) . .
C5 O2 H2 109.5 . .
Co1 O99 H99A 110.4 . .
Co1 O99 H99B 111.0 . .
H99A O99 H99B 107.9 . .
N91 Co1 N97 97.02(9) . .
N91 Co1 N94 170.58(9) . .
N97 Co1 N94 91.98(8) . .
N91 Co1 O99 86.97(7) . .
N97 Co1 O99 175.24(7) . .
N94 Co1 O99 84.17(7) . .
N91 Co1 N3 85.96(7) . .
N97 Co1 N3 91.42(7) . .
N94 Co1 N3 91.07(7) . .
O99 Co1 N3 91.45(7) . .
N91 Co1 N1 90.95(7) . .
N97 Co1 N1 86.15(7) . .
N94 Co1 N1 92.42(7) . .
O99 Co1 N1 91.20(7) . .
N3 Co1 N1 175.82(7) . .
N99 Co2 N99 180.0 2_565 .
N99 Co2 N96 90.37(9) 2_565 2
N99 Co2 N96 89.63(9) . 2
N99 Co2 N96 89.63(9) 2_565 1_565
N99 Co2 N96 90.37(9) . 1_565
N96 Co2 N96 180.00(12) 2 1_565
N99 Co2 N4 91.12(8) 2_565 2_565
N99 Co2 N4 88.88(8) . 2_565
N96 Co2 N4 88.43(8) 2 2_565
N96 Co2 N4 91.57(8) 1_565 2_565
N99 Co2 N4 88.88(8) 2_565 .
N99 Co2 N4 91.12(8) . .
N96 Co2 N4 91.58(8) 2 .
N96 Co2 N4 88.42(8) 1_565 .
N4 Co2 N4 180.0 2_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.302(3) .
C1 C2 1.439(3) .
C1 H1 0.9300 .
C2 O1 1.234(3) .
C2 N2 1.363(3) .
C3 C4 1.345(3) .
C3 N2 1.356(3) .
C3 H3 0.9300 .
C4 N1 1.375(3) .
C4 H4 0.9300 .
C5 N3 1.335(3) .
C5 O2 1.342(4) .
C5 C6 1.375(3) 2_755
C6 N3 1.332(3) .
C6 C5 1.375(3) 2_755
C6 H6 0.9300 .
C7 N4 1.303(3) .
C7 C8 1.434(3) .
C7 H7 0.9300 .
C8 O3 1.246(3) .
C8 N5 1.358(3) .
C9 C10 1.330(3) .
C9 N5 1.357(3) .
C9 H9 0.9300 .
C10 N4 1.368(3) .
C10 H10 0.9300 .
C94 N91 1.148(3) .
C94 N92 1.296(3) .
C95 N93 1.142(4) .
C95 N92 1.299(4) .
C96 N94 1.142(3) .
C96 N95 1.297(3) .
C97 N96 1.140(3) .
C97 N95 1.304(3) .
C98 N97 1.143(3) .
C98 N98 1.289(3) .
C99 N99 1.136(3) .
C99 N98 1.292(3) .
N1 Co1 2.2213(18) .
N2 H2N 0.84(3) .
N3 Co1 2.2024(18) .
N4 Co2 2.1868(19) .
N5 H5N 0.80(3) .
N91 Co1 2.056(2) .
N94 Co1 2.078(2) .
N96 Co2 2.114(2) 1_545
N97 Co1 2.071(2) .
N99 Co2 2.073(2) .
O2 H2 0.8200 .
O99 Co1 2.1653(16) .
O99 H99A 0.8744 .
O99 H99B 0.8748 .
Co2 N99 2.073(2) 2_565
Co2 N96 2.114(2) 2
Co2 N96 2.114(2) 1_565
Co2 N4 2.1868(19) 2_565
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O99 H99A O3 0.87 2.26 3.066(2) 153.5 1_645
N5 H5N N93 0.80(3) 2.21(3) 2.974(4) 161(3) 2_666
N2 H2N O3 0.84(3) 2.02(3) 2.813(3) 157(3) 2_566
C1 H1 N94 0.93 2.61 3.187(3) 120.9 .
C6 H6 N97 0.93 2.49 3.093(3) 122.5 .
O99 H99B O1 0.87 1.80 2.667(2) 170.3 1_655
