#------------------------------------------------------------------------------
#$Date: 2017-10-28 04:33:07 +0200 (Sat 28 de Oct de 2017) $
#$Revision: 202390 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/45/7044568.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_7044568
loop_
_publ_author_name
'Sethuraman, Muthuramalingam'
'Khamrang, Themmila'
'Velusamy, Marappan'
'Ramasamy, Mayilmurugan'
_publ_section_title
;
 Catalytic fixation of atmospheric carbon dioxide by copper(II) complexes
 of bidentate ligands
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03062B
_journal_year                    2017
_chemical_formula_sum            'C30 H26 Cl Cu N6 O4'
_chemical_formula_weight         633.56
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-08-08 deposited with the CCDC.
2017-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.588(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5802(11)
_cell_length_b                   14.7784(8)
_cell_length_c                   14.3077(11)
_cell_measurement_reflns_used    2858
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.370
_cell_measurement_theta_min      3.132
_cell_volume                     2803.4(4)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  EOS,Gemini
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6239
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.132
_exptl_absorpt_coefficient_mu    0.923
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       needle
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.058
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0757
_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)+(0.1568P)²+5.2328P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2196
_refine_ls_wR_factor_ref         0.2349
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2301
_reflns_number_total             2858
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt03062b2.cif
_cod_data_source_block           shelx_CCDC2
_cod_database_code               7044568
_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.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.5000 0.78461(6) 0.2500 0.0518(3) Uani 1 2 d S T P
Cl1 Cl 0.5000 0.11777(13) 0.2500 0.0619(5) Uani 1 2 d S T P
N3 N 0.5978(3) 0.8245(3) 0.1940(3) 0.0487(9) Uani 1 1 d . . .
N1 N 0.6235(3) 0.7123(2) 0.3466(3) 0.0400(7) Uani 1 1 d . . .
N2 N 0.8072(3) 0.6220(3) 0.4573(3) 0.0559(10) Uani 1 1 d . . .
C1 C 0.6375(3) 0.6617(3) 0.4315(3) 0.0410(9) Uani 1 1 d . . .
C8 C 0.7287(3) 0.6154(3) 0.4857(3) 0.0503(11) Uani 1 1 d . . .
C2 C 0.5607(3) 0.6564(3) 0.4666(4) 0.0485(10) Uani 1 1 d . . .
H2 H 0.5003 0.6870 0.4311 0.058 Uiso 1 1 calc R U .
C10 C 0.7010(3) 0.7188(3) 0.3210(3) 0.0425(9) Uani 1 1 d . . .
C9 C 0.7919(3) 0.6726(3) 0.3774(4) 0.0529(11) Uani 1 1 d . . .
H9 H 0.8441 0.6786 0.3566 0.064 Uiso 1 1 calc R U .
C11 C 0.6836(3) 0.7760(3) 0.2292(3) 0.0469(10) Uani 1 1 d . . .
C6 C 0.6637(5) 0.5568(3) 0.6039(4) 0.0597(13) Uani 1 1 d . . .
C3 C 0.5737(4) 0.6065(3) 0.5529(4) 0.0541(11) Uani 1 1 d . . .
C5 C 0.6774(6) 0.4973(4) 0.6948(5) 0.086(2) Uani 1 1 d . . .
H5A H 0.6180 0.5004 0.7079 0.129 Uiso 1 1 calc R U .
H5B H 0.7346 0.5179 0.7543 0.129 Uiso 1 1 calc R U .
H5C H 0.6883 0.4359 0.6799 0.129 Uiso 1 1 calc R U .
C7 C 0.7396(4) 0.5627(3) 0.5716(4) 0.0579(13) Uani 1 1 d . . .
H7 H 0.7994 0.5314 0.6070 0.070 Uiso 1 1 calc R U .
C13 C 0.7231(6) 0.8321(6) 0.0933(5) 0.087(2) Uani 1 1 d . . .
H13 H 0.7631 0.8327 0.0569 0.105 Uiso 1 1 calc R U .
C15 C 0.5770(4) 0.8777(4) 0.1109(4) 0.0664(14) Uani 1 1 d . . .
H15 H 0.5179 0.9116 0.0862 0.080 Uiso 1 1 calc R U .
C12 C 0.7490(5) 0.7776(4) 0.1812(5) 0.0713(15) Uani 1 1 d . . .
H12 H 0.8081 0.7437 0.2063 0.086 Uiso 1 1 calc R U .
C14 C 0.6388(6) 0.8836(5) 0.0623(5) 0.0821(19) Uani 1 1 d . . .
H14 H 0.6234 0.9233 0.0073 0.099 Uiso 1 1 calc R U .
C4 C 0.4908(5) 0.6071(4) 0.5905(5) 0.0743(16) Uani 1 1 d . . .
H4A H 0.5099 0.5693 0.6502 0.111 Uiso 1 1 calc R U .
H4B H 0.4295 0.5847 0.5373 0.111 Uiso 1 1 calc R U .
H4C H 0.4804 0.6679 0.6079 0.111 Uiso 1 1 calc R U .
O1 O 0.4845(13) 0.1895(11) 0.1880(10) 0.273(7) Uani 1 1 d . . .
O2 O 0.4234(14) 0.0852(10) 0.247(2) 0.452(17) 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'
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'
Cl Cl 0.1484 0.1585 '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
N3 Cu1 N3 145.6(2) . 2_655
N3 Cu1 N1 81.45(15) . .
N3 Cu1 N1 117.15(15) 2_655 .
N3 Cu1 N1 117.15(15) . 2_655
N3 Cu1 N1 81.45(15) 2_655 2_655
N1 Cu1 N1 117.37(18) . 2_655
O2 Cl1 O2 132.6(15) 2_655 .
O2 Cl1 O1 113.2(15) 2_655 2_655
O2 Cl1 O1 104.0(10) . 2_655
O2 Cl1 O1 104.0(10) 2_655 .
O2 Cl1 O1 113.2(15) . .
O1 Cl1 O1 75.5(14) 2_655 .
C11 N3 C15 118.2(4) . .
C11 N3 Cu1 113.6(3) . .
C15 N3 Cu1 126.2(4) . .
C10 N1 C1 117.0(3) . .
C10 N1 Cu1 112.6(3) . .
C1 N1 Cu1 130.3(3) . .
C9 N2 C8 116.3(4) . .
N1 C1 C2 120.0(4) . .
N1 C1 C8 120.9(4) . .
C2 C1 C8 119.1(4) . .
N2 C8 C7 119.7(4) . .
N2 C8 C1 121.1(4) . .
C7 C8 C1 119.2(5) . .
C3 C2 C1 121.0(4) . .
N1 C10 C9 120.8(4) . .
N1 C10 C11 115.5(4) . .
C9 C10 C11 123.6(4) . .
N2 C9 C10 123.8(4) . .
N3 C11 C12 121.9(5) . .
N3 C11 C10 115.0(4) . .
C12 C11 C10 123.0(5) . .
C7 C6 C3 120.0(5) . .
C7 C6 C5 119.5(5) . .
C3 C6 C5 120.5(6) . .
C2 C3 C6 119.4(5) . .
C2 C3 C4 118.8(5) . .
C6 C3 C4 121.8(5) . .
C6 C7 C8 121.2(4) . .
C14 C13 C12 119.0(5) . .
N3 C15 C14 122.6(6) . .
C11 C12 C13 117.9(6) . .
C15 C14 C13 120.2(6) . .
Cl1 O1 O1 52.3(7) . 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N3 1.994(4) .
Cu1 N3 1.994(4) 2_655
Cu1 N1 2.055(3) .
Cu1 N1 2.055(3) 2_655
Cl1 O2 1.199(8) 2_655
Cl1 O2 1.199(8) .
Cl1 O1 1.340(12) 2_655
Cl1 O1 1.340(12) .
N3 C11 1.345(6) .
N3 C15 1.350(6) .
N1 C10 1.329(6) .
N1 C1 1.368(5) .
N2 C9 1.305(7) .
N2 C8 1.368(6) .
C1 C2 1.406(6) .
C1 C8 1.407(6) .
C8 C7 1.406(7) .
C2 C3 1.383(6) .
C10 C9 1.409(6) .
C10 C11 1.492(7) .
C11 C12 1.389(7) .
C6 C7 1.368(8) .
C6 C3 1.413(8) .
C6 C5 1.512(7) .
C3 C4 1.514(8) .
C13 C14 1.354(11) .
C13 C12 1.406(10) .
C15 C14 1.350(9) .
O1 O1 1.64(3) 2_655
