#------------------------------------------------------------------------------
#$Date: 2019-11-23 22:10:59 +0200 (Sat, 23 Nov 2019) $
#$Revision: 235294 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/62/7236235.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_7236235
loop_
_publ_author_name
'Datta, Amitabha'
'Das, Kuheli'
'Mane, Sandeep B.'
'Mendiratta, Shruti'
'El Fallah, Mohamed Salah'
'Garribba, Eugenio'
'Bauzá, Antonio'
'Frontera, Antonio'
'Hung, Chen-Hsiung'
'Sinha, Chittaranjan'
_publ_section_title
;
 A rare doubly nitrato and phenoxido bridged trimetallic CuII complex:
 EPR, antiferromagnetic coupling and theoretical rationalization
;
_journal_issue                   60
_journal_name_full               'RSC Advances'
_journal_page_first              54856
_journal_paper_doi               10.1039/C6RA10674A
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         ' 'C34 H32 Cu3 N6 O10'
_chemical_formula_sum            'C34 H32 Cu3 N6 O10'
_chemical_formula_weight         875.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-04-18 deposited with the CCDC.
2016-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.034(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8854(4)
_cell_length_b                   11.6472(5)
_cell_length_c                   16.0930(6)
_cell_measurement_reflns_used    457
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      2.173
_cell_volume                     1634.68(12)
_computing_cell_refinement       'Bruker APEX-II (2008)'
_computing_data_collection       'Bruker APEX-II (2008)'
_computing_data_reduction        'Bruker SAINT (2008)'
_computing_molecular_graphics    'Mercury CSD 3.6'
_computing_publication_material
'SHELXL and WINGX (Farrugia, J. App. Cryst.2012, 45, 849-854'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0963
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            56645
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.173
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.006
_exptl_absorpt_correction_T_max  0.9705
_exptl_absorpt_correction_T_min  0.8871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS, 1996'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             890
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.0006(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0275P)²+2.0803P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2990
_reflns_number_total             3619
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ra10674a2.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7236235
_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.27673(3) 0.68418(3) 0.44151(2) 0.01054(10) Uani 1 1 d . . .
Cu2 Cu 0.5000 0.5000 0.5000 0.01028(11) Uani 1 2 d S . P
O1 O 0.32198(19) 0.57421(14) 0.53464(10) 0.0121(4) Uani 1 1 d . . .
O2 O 0.39371(19) 0.56924(14) 0.39363(10) 0.0121(4) Uani 1 1 d . . .
O3 O 0.4781(2) 0.80638(15) 0.49623(11) 0.0172(4) Uani 1 1 d . . .
O4 O 0.6452(2) 0.67143(15) 0.53915(12) 0.0168(4) Uani 1 1 d . . .
O5 O 0.7131(2) 0.85029(16) 0.55234(13) 0.0231(4) Uani 1 1 d . . .
N1 N 0.1125(2) 0.75655(18) 0.48890(13) 0.0123(4) Uani 1 1 d . . .
N2 N 0.2600(2) 0.78007(17) 0.34086(13) 0.0118(4) Uani 1 1 d . . .
N3 N 0.6126(2) 0.77650(18) 0.52946(13) 0.0135(5) Uani 1 1 d . . .
C1 C 0.0589(3) 0.8744(2) 0.46490(16) 0.0159(5) Uani 1 1 d . . .
H1A H 0.1257 0.9294 0.5018 0.019 Uiso 1 1 calc R U .
H1B H -0.0462 0.8833 0.4761 0.019 Uiso 1 1 calc R U .
C2 C 0.0573(3) 0.9062(2) 0.37320(16) 0.0160(5) Uani 1 1 d . . .
H2A H 0.0168 0.9852 0.3630 0.019 Uiso 1 1 calc R U .
H2B H -0.0133 0.8539 0.3360 0.019 Uiso 1 1 calc R U .
C3 C 0.2145(3) 0.9002(2) 0.34895(17) 0.0156(5) Uani 1 1 d . . .
H3B H 0.2116 0.9406 0.2945 0.019 Uiso 1 1 calc R U .
H3A H 0.2910 0.9391 0.3928 0.019 Uiso 1 1 calc R U .
C4 C 0.0415(3) 0.7027(2) 0.53944(15) 0.0135(5) Uani 1 1 d . . .
H4 H -0.0478 0.7388 0.5514 0.016 Uiso 1 1 calc R U .
C5 C 0.0821(3) 0.5929(2) 0.58030(15) 0.0115(5) Uani 1 1 d . . .
C6 C 0.2187(3) 0.5326(2) 0.57768(15) 0.0115(5) Uani 1 1 d . . .
C7 C 0.2473(3) 0.4290(2) 0.62271(15) 0.0134(5) Uani 1 1 d . . .
H7 H 0.3378 0.3867 0.6203 0.016 Uiso 1 1 calc R U .
C8 C 0.1449(3) 0.3882(2) 0.67046(15) 0.0146(5) Uani 1 1 d . . .
H8 H 0.1671 0.3190 0.7016 0.018 Uiso 1 1 calc R U .
C9 C 0.0097(3) 0.4471(2) 0.67350(16) 0.0163(5) Uani 1 1 d . . .
H9 H -0.0605 0.4182 0.7061 0.020 Uiso 1 1 calc R U .
C10 C -0.0210(3) 0.5479(2) 0.62876(15) 0.0137(5) Uani 1 1 d . . .
H10 H -0.1135 0.5880 0.6305 0.016 Uiso 1 1 calc R U .
C11 C 0.2948(3) 0.7483(2) 0.27070(16) 0.0135(5) Uani 1 1 d . . .
H11 H 0.2894 0.8051 0.2279 0.016 Uiso 1 1 calc R U .
C12 C 0.3417(3) 0.6339(2) 0.25018(15) 0.0129(5) Uani 1 1 d . . .
C13 C 0.3820(3) 0.5459(2) 0.31089(15) 0.0116(5) Uani 1 1 d . . .
C14 C 0.4097(3) 0.4357(2) 0.28279(16) 0.0148(5) Uani 1 1 d . . .
H14 H 0.4322 0.3748 0.3225 0.018 Uiso 1 1 calc R U .
C15 C 0.4046(3) 0.4147(2) 0.19791(17) 0.0183(6) Uani 1 1 d . . .
H15 H 0.4199 0.3387 0.1799 0.022 Uiso 1 1 calc R U .
C16 C 0.3774(3) 0.5023(2) 0.13824(17) 0.0195(6) Uani 1 1 d . . .
H16 H 0.3802 0.4878 0.0805 0.023 Uiso 1 1 calc R U .
C17 C 0.3465(3) 0.6104(2) 0.16488(16) 0.0176(6) Uani 1 1 d . . .
H17 H 0.3278 0.6710 0.1246 0.021 Uiso 1 1 calc R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
O2 Cu1 N2 91.53(8) . .
O2 Cu1 O1 78.77(7) . .
N2 Cu1 O1 169.92(8) . .
O2 Cu1 N1 160.88(8) . .
N2 Cu1 N1 97.63(9) . .
O1 Cu1 N1 92.45(8) . .
O2 Cu1 O3 98.09(7) . .
N2 Cu1 O3 83.95(8) . .
O1 Cu1 O3 94.61(7) . .
N1 Cu1 O3 99.53(8) . .
O2 Cu1 Cu2 41.19(5) . .
N2 Cu1 Cu2 128.39(6) . .
O1 Cu1 Cu2 41.56(5) . .
N1 Cu1 Cu2 133.88(6) . .
O3 Cu1 Cu2 84.40(4) . .
O2 Cu2 O2 180.00(9) 3_666 .
O2 Cu2 O1 102.20(7) 3_666 .
O2 Cu2 O1 77.80(7) . .
O2 Cu2 O1 77.80(7) 3_666 3_666
O2 Cu2 O1 102.20(7) . 3_666
O1 Cu2 O1 180.00(14) . 3_666
O2 Cu2 O4 91.83(7) 3_666 3_666
O2 Cu2 O4 88.17(7) . 3_666
O1 Cu2 O4 91.08(7) . 3_666
O1 Cu2 O4 88.92(7) 3_666 3_666
O2 Cu2 O4 88.17(7) 3_666 .
O2 Cu2 O4 91.83(7) . .
O1 Cu2 O4 88.92(7) . .
O1 Cu2 O4 91.08(7) 3_666 .
O4 Cu2 O4 180.0 3_666 .
O2 Cu2 Cu1 40.66(5) 3_666 3_666
O2 Cu2 Cu1 139.34(5) . 3_666
O1 Cu2 Cu1 138.96(5) . 3_666
O1 Cu2 Cu1 41.04(5) 3_666 3_666
O4 Cu2 Cu1 76.90(4) 3_666 3_666
O4 Cu2 Cu1 103.10(4) . 3_666
O2 Cu2 Cu1 139.34(5) 3_666 .
O2 Cu2 Cu1 40.66(5) . .
O1 Cu2 Cu1 41.04(5) . .
O1 Cu2 Cu1 138.96(5) 3_666 .
O4 Cu2 Cu1 103.10(4) 3_666 .
O4 Cu2 Cu1 76.90(4) . .
Cu1 Cu2 Cu1 180.0 3_666 .
C6 O1 Cu1 124.89(15) . .
C6 O1 Cu2 130.68(15) . .
Cu1 O1 Cu2 97.40(7) . .
C13 O2 Cu1 125.94(15) . .
C13 O2 Cu2 135.58(15) . .
Cu1 O2 Cu2 98.15(7) . .
N3 O3 Cu1 126.16(15) . .
N3 O4 Cu2 132.61(15) . .
C4 N1 C1 116.4(2) . .
C4 N1 Cu1 121.93(17) . .
C1 N1 Cu1 121.57(16) . .
C11 N2 C3 118.1(2) . .
C11 N2 Cu1 125.02(18) . .
C3 N2 Cu1 116.78(16) . .
O5 N3 O4 119.9(2) . .
O5 N3 O3 120.2(2) . .
O4 N3 O3 119.8(2) . .
N1 C1 C2 115.0(2) . .
N1 C1 H1A 108.5 . .
C2 C1 H1A 108.5 . .
N1 C1 H1B 108.5 . .
C2 C1 H1B 108.5 . .
H1A C1 H1B 107.5 . .
C1 C2 C3 113.5(2) . .
C1 C2 H2A 108.9 . .
C3 C2 H2A 108.9 . .
C1 C2 H2B 108.9 . .
C3 C2 H2B 108.9 . .
H2A C2 H2B 107.7 . .
N2 C3 C2 110.4(2) . .
N2 C3 H3B 109.6 . .
C2 C3 H3B 109.6 . .
N2 C3 H3A 109.6 . .
C2 C3 H3A 109.6 . .
H3B C3 H3A 108.1 . .
N1 C4 C5 127.4(2) . .
N1 C4 H4 116.3 . .
C5 C4 H4 116.3 . .
C6 C5 C10 119.0(2) . .
C6 C5 C4 124.5(2) . .
C10 C5 C4 116.5(2) . .
O1 C6 C7 120.1(2) . .
O1 C6 C5 120.9(2) . .
C7 C6 C5 119.0(2) . .
C8 C7 C6 120.6(2) . .
C8 C7 H7 119.7 . .
C6 C7 H7 119.7 . .
C7 C8 C9 120.9(2) . .
C7 C8 H8 119.5 . .
C9 C8 H8 119.5 . .
C10 C9 C8 119.2(2) . .
C10 C9 H9 120.4 . .
C8 C9 H9 120.4 . .
C9 C10 C5 121.4(2) . .
C9 C10 H10 119.3 . .
C5 C10 H10 119.3 . .
N2 C11 C12 126.4(2) . .
N2 C11 H11 116.8 . .
C12 C11 H11 116.8 . .
C17 C12 C13 118.8(2) . .
C17 C12 C11 117.6(2) . .
C13 C12 C11 123.6(2) . .
O2 C13 C14 121.4(2) . .
O2 C13 C12 119.9(2) . .
C14 C13 C12 118.6(2) . .
C15 C14 C13 120.6(2) . .
C15 C14 H14 119.7 . .
C13 C14 H14 119.7 . .
C14 C15 C16 121.5(3) . .
C14 C15 H15 119.3 . .
C16 C15 H15 119.3 . .
C17 C16 C15 118.4(2) . .
C17 C16 H16 120.8 . .
C15 C16 H16 120.8 . .
C16 C17 C12 121.8(2) . .
C16 C17 H17 119.1 . .
C12 C17 H17 119.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O2 1.9425(17) .
Cu1 N2 1.950(2) .
Cu1 O1 1.9539(17) .
Cu1 N1 1.961(2) .
Cu1 O3 2.3239(18) .
Cu1 Cu2 2.9511(3) .
Cu2 O2 1.9632(16) 3_666
Cu2 O2 1.9632(16) .
Cu2 O1 1.9742(16) .
Cu2 O1 1.9742(16) 3_666
Cu2 O4 2.3953(18) 3_666
Cu2 O4 2.3953(18) .
Cu2 Cu1 2.9511(3) 3_666
O1 C6 1.342(3) .
O2 C13 1.343(3) .
O3 N3 1.261(3) .
O4 N3 1.261(3) .
O5 N3 1.243(3) .
N1 C4 1.285(3) .
N1 C1 1.479(3) .
N2 C11 1.281(3) .
N2 C3 1.470(3) .
C1 C2 1.519(4) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C3 1.522(3) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3B 0.9900 .
C3 H3A 0.9900 .
C4 C5 1.452(3) .
C4 H4 0.9500 .
C5 C6 1.410(3) .
C5 C10 1.413(3) .
C6 C7 1.405(3) .
C7 C8 1.383(3) .
C7 H7 0.9500 .
C8 C9 1.393(4) .
C8 H8 0.9500 .
C9 C10 1.376(4) .
C9 H9 0.9500 .
C10 H10 0.9500 .
C11 C12 1.452(4) .
C11 H11 0.9500 .
C12 C17 1.408(3) .
C12 C13 1.414(3) .
C13 C14 1.397(4) .
C14 C15 1.380(4) .
C14 H14 0.9500 .
C15 C16 1.390(4) .
C15 H15 0.9500 .
C16 C17 1.376(4) .
C16 H16 0.9500 .
C17 H17 0.9500 .
