#------------------------------------------------------------------------------
#$Date: 2017-07-22 05:02:34 +0300 (Sat, 22 Jul 2017) $
#$Revision: 198908 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/37/7043736.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_7043736
loop_
_publ_author_name
'Palacios, Maria A.'
'Morlieras, Jessica'
'Herrera, Juan Manuel'
'Mota, Antonio J.'
'Brechin, Euan K.'
'Triki, Smail'
'Colacio, Enrique'
_publ_section_title
;
 Synthetic ability of dinuclear mesocates containing
 1,3-bis(diazinecarboxamide)benzene bridging ligands to form complexes of
 increased nuclearity. Crystal structures, magnetic properties and
 theoretical studies.
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02288C
_journal_year                    2017
_chemical_formula_moiety         'C32 H24 Cu2 N12 O6, 2(H2 O)'
_chemical_formula_sum            'C32 H28 Cu2 N12 O8'
_chemical_formula_weight         835.74
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-17 deposited with the CCDC.
2017-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                116.889(5)
_cell_angle_beta                 100.695(5)
_cell_angle_gamma                101.227(5)
_cell_formula_units_Z            1
_cell_length_a                   7.6178(19)
_cell_length_b                   11.658(3)
_cell_length_c                   11.819(3)
_cell_measurement_reflns_used    16527
_cell_measurement_temperature    100
_cell_measurement_theta_max      40.522
_cell_measurement_theta_min      5.907
_cell_volume                     872.2(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_unetI/netI     0.1197
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.870
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5403
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.051
_diffrn_reflns_theta_min         2.034
_exptl_absorpt_coefficient_mu    1.289
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.361400
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SAD V2.05 (?, 2016) was used for absorption correction.
R(int) was 0.0581 before and 0.0282 after correction.
The Ratio of minimum to maximum transmission is 0.3614.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'metallic greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       plate
_exptl_crystal_F_000             426
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.662
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1195
_refine_ls_R_factor_gt           0.0807
_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)+(0.1068P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.2182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2292
_reflns_number_total             3682
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt02288c2.cif
_cod_data_source_block           hastalli
_cod_database_code               7043736
_shelxl_version_number           2013-4
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O2W(0.5) H2WA(0.5) H2WB(0.5) O1W(0.5) H1WA(0.5) H1WB(0.5)
3.a Free rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
3.b Rotating group:
 O1(H1A,H1B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15),
 C16(H16)
;
_olex2_submission_special_instructions 'No special instructions were received'
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_occupancy
Cu1 Cu 0.20966(10) 0.37999(7) 0.17015(7) 0.0371(3) Uani 1 1 d . .
O1 O 0.0579(6) 0.5015(4) 0.2734(4) 0.0442(11) Uani 1 1 d . .
H1A H 0.0380 0.5481 0.2194 0.066 Uiso 1 1 d GR .
H1B H -0.0555 0.4517 0.2607 0.066 Uiso 1 1 d GR .
O2 O -0.0020(6) 0.3041(4) -0.2070(4) 0.0430(10) Uani 1 1 d . .
O3 O 0.7334(6) 0.3558(5) 0.2789(5) 0.0539(12) Uani 1 1 d . .
N1 N -0.0341(7) 0.2057(5) 0.0340(5) 0.0399(12) Uani 1 1 d . .
N2 N -0.3246(10) -0.0135(6) -0.1836(7) 0.0651(18) Uani 1 1 d . .
N3 N 0.1571(6) 0.4130(5) 0.0189(5) 0.0328(11) Uani 1 1 d . .
N4 N 0.4585(7) 0.3570(5) 0.1569(5) 0.0352(11) Uani 1 1 d . .
N5 N 0.2837(7) 0.3469(5) 0.3227(5) 0.0380(12) Uani 1 1 d . .
N6 N 0.4367(9) 0.3038(7) 0.5268(6) 0.0588(16) Uani 1 1 d . .
C1 C -0.1381(10) 0.1057(7) 0.0437(7) 0.0509(18) Uani 1 1 d . .
H1 H -0.1133 0.1088 0.1270 0.061 Uiso 1 1 calc R .
C2 C -0.2807(11) -0.0016(7) -0.0655(8) 0.057(2) Uani 1 1 d . .
H2 H -0.3508 -0.0706 -0.0545 0.069 Uiso 1 1 calc R .
C3 C -0.2186(10) 0.0888(7) -0.1923(7) 0.0517(18) Uani 1 1 d . .
H3 H -0.2442 0.0854 -0.2757 0.062 Uiso 1 1 calc R .
C4 C -0.0773(8) 0.1957(6) -0.0858(6) 0.0364(14) Uani 1 1 d . .
C5 C 0.0341(8) 0.3130(6) -0.0951(6) 0.0353(13) Uani 1 1 d . .
C6 C 0.2823(8) 0.5284(6) 0.0299(6) 0.0310(12) Uani 1 1 d . .
C7 C 0.3765(9) 0.6385(6) 0.1608(6) 0.0359(13) Uani 1 1 d . .
H7 H 0.3458 0.6364 0.2343 0.043 Uiso 1 1 calc R .
C8 C 0.5122(9) 0.7484(6) 0.1819(6) 0.0406(14) Uani 1 1 d . .
H8 H 0.5737 0.8226 0.2703 0.049 Uiso 1 1 calc R .
C9 C 0.3320(8) 0.5337(6) -0.0749(6) 0.0314(12) Uani 1 1 d . .
H9 H 0.2697 0.4607 -0.1638 0.038 Uiso 1 1 calc R .
C10 C 0.4384(9) 0.2464(6) -0.0771(6) 0.0419(15) Uani 1 1 d . .
H10 H 0.3444 0.1693 -0.0930 0.050 Uiso 1 1 calc R .
C11 C 0.5275(8) 0.3547(6) 0.0508(6) 0.0339(13) Uani 1 1 d . .
C12 C 0.5672(9) 0.3549(6) 0.2575(6) 0.0373(14) Uani 1 1 d . .
C13 C 0.4611(9) 0.3433(5) 0.3492(6) 0.0364(14) Uani 1 1 d . .
C14 C 0.5355(10) 0.3223(7) 0.4516(7) 0.0471(16) Uani 1 1 d . .
H14 H 0.6618 0.3211 0.4687 0.057 Uiso 1 1 calc R .
C15 C 0.2592(12) 0.3075(7) 0.4982(7) 0.059(2) Uani 1 1 d . .
H15 H 0.1832 0.2925 0.5486 0.070 Uiso 1 1 calc R .
C16 C 0.1828(10) 0.3319(7) 0.4002(7) 0.0472(16) Uani 1 1 d . .
H16 H 0.0589 0.3381 0.3868 0.057 Uiso 1 1 calc R .
O2W O -0.2256(16) 0.0956(11) 0.2995(11) 0.074(4) Uani 0.5 1 d . P
H2WA H -0.3300 0.0645 0.3078 0.112 Uiso 0.5 1 d G P
H2WB H -0.1600 0.1693 0.3712 0.112 Uiso 0.5 1 d G P
O1W O -0.1049(15) 0.0870(10) -0.4716(9) 0.063(3) Uani 0.5 1 d . P
H1WA H -0.1858 0.1071 -0.5159 0.095 Uiso 0.5 1 d G P
H1WB H -0.0987 0.1282 -0.3878 0.095 Uiso 0.5 1 d G 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'
Cu Cu 0.3201 1.2651 '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
O1 Cu1 N1 95.24(18) . .
N3 Cu1 O1 94.64(18) . .
N3 Cu1 N1 80.26(19) . .
N3 Cu1 N4 94.62(19) . .
N3 Cu1 N5 175.4(2) . .
N4 Cu1 O1 148.21(19) . .
N4 Cu1 N1 116.3(2) . .
N4 Cu1 N5 80.9(2) . .
N5 Cu1 O1 88.97(19) . .
N5 Cu1 N1 102.20(19) . .
Cu1 O1 H1A 99.0 . .
Cu1 O1 H1B 111.4 . .
H1A O1 H1B 106.3 . .
C1 N1 Cu1 133.4(5) . .
C4 N1 Cu1 109.9(4) . .
C4 N1 C1 116.6(6) . .
C2 N2 C3 115.1(6) . .
C5 N3 Cu1 117.3(4) . .
C5 N3 C6 123.0(5) . .
C6 N3 Cu1 118.1(4) . .
C11 N4 Cu1 122.5(4) . .
C12 N4 Cu1 116.8(4) . .
C12 N4 C11 120.5(5) . .
C13 N5 Cu1 113.0(4) . .
C13 N5 C16 117.9(5) . .
C16 N5 Cu1 129.1(5) . .
C14 N6 C15 116.0(6) . .
N1 C1 H1 119.6 . .
N1 C1 C2 120.9(6) . .
C2 C1 H1 119.6 . .
N2 C2 C1 123.5(6) . .
N2 C2 H2 118.2 . .
C1 C2 H2 118.2 . .
N2 C3 H3 118.8 . .
N2 C3 C4 122.4(7) . .
C4 C3 H3 118.8 . .
N1 C4 C3 121.5(6) . .
N1 C4 C5 116.5(5) . .
C3 C4 C5 121.9(6) . .
O2 C5 N3 128.2(5) . .
O2 C5 C4 117.3(5) . .
N3 C5 C4 114.4(5) . .
C7 C6 N3 115.9(5) . .
C9 C6 N3 125.1(5) . .
C9 C6 C7 118.6(5) . .
C6 C7 H7 120.0 . .
C8 C7 C6 120.0(5) . .
C8 C7 H7 120.0 . .
C7 C8 H8 119.4 . .
C7 C8 C10 121.3(6) . 2_665
C10 C8 H8 119.4 2_665 .
C6 C9 H9 119.8 . .
C6 C9 C11 120.4(5) . 2_665
C11 C9 H9 119.8 2_665 .
C8 C10 H10 120.5 2_665 .
C11 C10 C8 119.0(6) . 2_665
C11 C10 H10 120.5 . .
C9 C11 N4 120.2(5) 2_665 .
C10 C11 N4 118.8(5) . .
C10 C11 C9 120.7(5) . 2_665
O3 C12 N4 128.7(6) . .
O3 C12 C13 119.6(6) . .
N4 C12 C13 111.6(5) . .
N5 C13 C12 116.6(5) . .
N5 C13 C14 120.6(6) . .
C14 C13 C12 122.7(6) . .
N6 C14 C13 122.3(7) . .
N6 C14 H14 118.8 . .
C13 C14 H14 118.8 . .
N6 C15 H15 118.4 . .
N6 C15 C16 123.2(7) . .
C16 C15 H15 118.4 . .
N5 C16 C15 119.8(7) . .
N5 C16 H16 120.1 . .
C15 C16 H16 120.1 . .
H2WA O2W H2WB 109.5 . .
H1WA O1W H1WB 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 2.105(4) .
Cu1 N1 2.152(5) .
Cu1 N3 1.980(5) .
Cu1 N4 1.990(5) .
Cu1 N5 2.013(5) .
O1 H1A 1.0172 .
O1 H1B 0.8856 .
O2 C5 1.251(7) .
O3 C12 1.241(7) .
N1 C1 1.340(8) .
N1 C4 1.338(8) .
N2 C2 1.308(9) .
N2 C3 1.360(8) .
N3 C5 1.318(7) .
N3 C6 1.426(7) .
N4 C11 1.438(7) .
N4 C12 1.330(8) .
N5 C13 1.343(8) .
N5 C16 1.348(8) .
N6 C14 1.327(9) .
N6 C15 1.346(10) .
C1 H1 0.9500 .
C1 C2 1.379(10) .
C2 H2 0.9500 .
C3 H3 0.9500 .
C3 C4 1.361(8) .
C4 C5 1.523(8) .
C6 C7 1.410(8) .
C6 C9 1.385(8) .
C7 H7 0.9500 .
C7 C8 1.368(8) .
C8 H8 0.9500 .
C8 C10 1.382(8) 2_665
C9 H9 0.9500 .
C9 C11 1.389(8) 2_665
C10 C8 1.382(8) 2_665
C10 H10 0.9500 .
C10 C11 1.378(8) .
C11 C9 1.389(8) 2_665
C12 C13 1.504(8) .
C13 C14 1.383(8) .
C14 H14 0.9500 .
C15 H15 0.9500 .
C15 C16 1.369(10) .
C16 H16 0.9500 .
O2W H2WA 0.8498 .
O2W H2WB 0.8503 .
O1W H1WA 0.8699 .
O1W H1WB 0.8699 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Cu1 N1 C1 C2 -174.5(5) . .
Cu1 N1 C4 C3 175.6(5) . .
Cu1 N1 C4 C5 -7.0(6) . .
Cu1 N3 C5 O2 -169.5(5) . .
Cu1 N3 C5 C4 11.0(7) . .
Cu1 N3 C6 C7 -27.5(6) . .
Cu1 N3 C6 C9 145.0(5) . .
Cu1 N4 C11 C9 105.0(6) . 2_665
Cu1 N4 C11 C10 -68.2(6) . .
Cu1 N4 C12 O3 -171.9(5) . .
Cu1 N4 C12 C13 11.2(6) . .
Cu1 N5 C13 C12 -3.8(6) . .
Cu1 N5 C13 C14 179.6(4) . .
Cu1 N5 C16 C15 178.8(5) . .
O3 C12 C13 N5 178.1(5) . .
O3 C12 C13 C14 -5.5(9) . .
N1 C1 C2 N2 -0.3(12) . .
N1 C4 C5 O2 178.6(5) . .
N1 C4 C5 N3 -1.9(8) . .
N2 C3 C4 N1 0.3(11) . .
N2 C3 C4 C5 -177.0(7) . .
N3 C6 C7 C8 173.9(6) . .
N3 C6 C9 C11 -172.1(5) . 2_665
N4 C12 C13 N5 -4.6(7) . .
N4 C12 C13 C14 171.8(5) . .
N5 C13 C14 N6 0.6(10) . .
N6 C15 C16 N5 3.2(11) . .
C1 N1 C4 C3 -0.6(9) . .
C1 N1 C4 C5 176.9(6) . .
C2 N2 C3 C4 0.0(11) . .
C3 N2 C2 C1 0.0(12) . .
C3 C4 C5 O2 -4.0(9) . .
C3 C4 C5 N3 175.5(6) . .
C4 N1 C1 C2 0.5(10) . .
C5 N3 C6 C7 167.2(5) . .
C5 N3 C6 C9 -20.3(9) . .
C6 N3 C5 O2 -4.1(10) . .
C6 N3 C5 C4 176.4(5) . .
C6 C7 C8 C10 -0.8(10) . 2_665
C7 C6 C9 C11 0.3(8) . 2_665
C8 C10 C11 N4 171.7(6) 2_665 .
C8 C10 C11 C9 -1.5(9) 2_665 2_665
C9 C6 C7 C8 0.8(9) . .
C11 N4 C12 O3 2.9(10) . .
C11 N4 C12 C13 -174.1(5) . .
C12 N4 C11 C9 -69.4(8) . 2_665
C12 N4 C11 C10 117.4(6) . .
C12 C13 C14 N6 -175.7(6) . .
C13 N5 C16 C15 -2.9(9) . .
C14 N6 C15 C16 -1.5(11) . .
C15 N6 C14 C13 -0.4(10) . .
C16 N5 C13 C12 177.6(5) . .
C16 N5 C13 C14 1.1(8) . .
