#------------------------------------------------------------------------------
#$Date: 2016-05-06 05:08:28 +0300 (Fri, 06 May 2016) $
#$Revision: 182773 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/53/7055348.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_7055348
loop_
_publ_author_name
'Patra, Shanti G.'
'Shee, Nirmal K.'
'Drew, Michael G. B.'
'Datta, Dipankar'
_publ_section_title
;
 Angle isomerism, as exemplified in a five-coordinate, dimeric copper(ii)
 Schiff base complex. Observation of Ostwald ripening
;
_journal_issue                   4
_journal_name_full               'New J. Chem.'
_journal_page_first              3238
_journal_paper_doi               10.1039/C5NJ02765A
_journal_volume                  40
_journal_year                    2016
_chemical_formula_sum            'C38 H28 Cl2 Cu2 N6 O2'
_chemical_formula_weight         798.64
_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
_audit_update_record
;
2016-01-14 deposited with the CCDC.
2016-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                99.208(6)
_cell_angle_beta                 95.428(6)
_cell_angle_gamma                108.174(7)
_cell_formula_units_Z            1
_cell_length_a                   7.1801(6)
_cell_length_b                   10.2796(7)
_cell_length_c                   12.3788(8)
_cell_measurement_reflns_used    6030
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.97
_cell_volume                     846.66(12)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL, PLATON, WINGX (Ferrugia, 2012)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_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  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6030
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    1.459
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             406
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0405P)²+0.2894P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0899
_reflns_number_gt                4115
_reflns_number_total             4734
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj02765a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7055347--7055348.cif.'
_cod_original_cell_volume        846.66(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7055348
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
Cu1 Cu 0.96362(3) 0.39987(3) 0.377900(18) 0.01821(8) Uani 1 1 d .
Cl1 Cl 1.15982(7) 0.40117(5) 0.53040(4) 0.02106(11) Uani 1 1 d .
N11 N 1.1595(2) 0.51841(18) 0.30080(13) 0.0202(3) Uani 1 1 d .
C12 C 1.3507(3) 0.5952(2) 0.33833(18) 0.0256(4) Uani 1 1 d .
H12 H 1.4097 0.5875 0.4061 0.031 Uiso 1 1 calc R
C13 C 1.4614(3) 0.6853(2) 0.27860(19) 0.0297(5) Uani 1 1 d .
H13 H 1.5939 0.7367 0.3054 0.036 Uiso 1 1 calc R
C14 C 1.3730(3) 0.6983(2) 0.17810(18) 0.0259(4) Uani 1 1 d .
H14 H 1.4449 0.7600 0.1377 0.031 Uiso 1 1 calc R
C15 C 1.1776(3) 0.6190(2) 0.13869(17) 0.0222(4) Uani 1 1 d .
H15 H 1.1164 0.6255 0.0711 0.027 Uiso 1 1 calc R
C16 C 1.0735(3) 0.5292(2) 0.20189(16) 0.0183(4) Uani 1 1 d .
N17 N 0.8759(2) 0.44595(18) 0.16189(13) 0.0191(3) Uani 1 1 d .
N18 N 0.8025(2) 0.37512(17) 0.23489(13) 0.0167(3) Uani 1 1 d .
C19 C 0.6189(3) 0.2835(2) 0.22019(15) 0.0174(4) Uani 1 1 d .
C20 C 0.5841(3) 0.2209(2) 0.31553(15) 0.0178(4) Uani 1 1 d .
O21 O 0.7242(2) 0.24718(15) 0.39484(11) 0.0219(3) Uani 1 1 d .
C41 C 0.3885(3) 0.1249(2) 0.32724(15) 0.0186(4) Uani 1 1 d .
C42 C 0.2121(3) 0.1504(2) 0.29824(17) 0.0238(4) Uani 1 1 d .
H42 H 0.2133 0.2252 0.2645 0.029 Uiso 1 1 calc R
C43 C 0.0356(3) 0.0633(2) 0.32016(18) 0.0286(5) Uani 1 1 d .
H43 H -0.0816 0.0813 0.3028 0.034 Uiso 1 1 calc R
C44 C 0.0322(3) -0.0504(3) 0.36770(18) 0.0310(5) Uani 1 1 d .
H44 H -0.0872 -0.1082 0.3822 0.037 Uiso 1 1 calc R
C45 C 0.2053(3) -0.0783(2) 0.39357(19) 0.0320(5) Uani 1 1 d .
H45 H 0.2022 -0.1565 0.4232 0.038 Uiso 1 1 calc R
C46 C 0.3832(3) 0.0105(2) 0.37522(18) 0.0269(4) Uani 1 1 d .
H46 H 0.5004 -0.0063 0.3951 0.032 Uiso 1 1 calc R
C31 C 0.4725(3) 0.2506(2) 0.11910(15) 0.0173(4) Uani 1 1 d .
C32 C 0.3790(3) 0.1127(2) 0.06300(16) 0.0215(4) Uani 1 1 d .
H32 H 0.4145 0.0411 0.0867 0.026 Uiso 1 1 calc R
C33 C 0.4193(3) 0.3567(2) 0.08112(17) 0.0216(4) Uani 1 1 d .
H33 H 0.4830 0.4493 0.1168 0.026 Uiso 1 1 calc R
C34 C 0.2721(3) 0.3252(2) -0.00946(17) 0.0251(4) Uani 1 1 d .
H34 H 0.2368 0.3965 -0.0339 0.030 Uiso 1 1 calc R
C35 C 0.1774(3) 0.1873(2) -0.06359(17) 0.0265(4) Uani 1 1 d .
H35 H 0.0769 0.1661 -0.1234 0.032 Uiso 1 1 calc R
C36 C 0.2326(3) 0.0819(2) -0.02853(17) 0.0253(4) Uani 1 1 d .
H36 H 0.1718 -0.0101 -0.0662 0.030 Uiso 1 1 calc R
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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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
N18 Cu1 N11 78.97(7) .
N18 Cu1 O21 80.93(6) .
N11 Cu1 O21 157.90(6) .
N18 Cu1 Cl1 171.57(5) .
N11 Cu1 Cl1 100.84(5) .
O21 Cu1 Cl1 97.70(4) .
N18 Cu1 Cl1 92.65(5) 2_766
N11 Cu1 Cl1 95.96(5) 2_766
O21 Cu1 Cl1 94.05(5) 2_766
Cl1 Cu1 Cl1 95.745(18) 2_766
Cu1 Cl1 Cu1 84.255(18) 2_766
C12 N11 C16 119.28(18) .
C12 N11 Cu1 128.86(14) .
C16 N11 Cu1 111.50(12) .
N11 C12 C13 121.6(2) .
N11 C12 H12 119.2 .
C13 C12 H12 119.2 .
C12 C13 C14 119.31(19) .
C12 C13 H13 120.3 .
C14 C13 H13 120.3 .
C15 C14 C13 119.4(2) .
C15 C14 H14 120.3 .
C13 C14 H14 120.3 .
C14 C15 C16 118.82(19) .
C14 C15 H15 120.6 .
C16 C15 H15 120.6 .
N11 C16 C15 121.59(17) .
N11 C16 N17 118.96(17) .
C15 C16 N17 119.45(17) .
N18 N17 C16 110.01(15) .
N17 N18 C19 124.42(16) .
N17 N18 Cu1 119.99(12) .
C19 N18 Cu1 115.59(13) .
N18 C19 C20 110.87(16) .
N18 C19 C31 124.34(17) .
C20 C19 C31 124.79(17) .
O21 C20 C19 120.22(17) .
O21 C20 C41 116.74(17) .
C19 C20 C41 123.04(16) .
C20 O21 Cu1 111.72(12) .
C46 C41 C42 119.47(19) .
C46 C41 C20 118.25(17) .
C42 C41 C20 122.16(18) .
C43 C42 C41 119.4(2) .
C43 C42 H42 120.3 .
C41 C42 H42 120.3 .
C44 C43 C42 120.6(2) .
C44 C43 H43 119.7 .
C42 C43 H43 119.7 .
C45 C44 C43 120.2(2) .
C45 C44 H44 119.9 .
C43 C44 H44 119.9 .
C44 C45 C46 119.6(2) .
C44 C45 H45 120.2 .
C46 C45 H45 120.2 .
C45 C46 C41 120.7(2) .
C45 C46 H46 119.7 .
C41 C46 H46 119.7 .
C32 C31 C33 119.04(17) .
C32 C31 C19 120.62(17) .
C33 C31 C19 120.28(17) .
C36 C32 C31 120.18(19) .
C36 C32 H32 119.9 .
C31 C32 H32 119.9 .
C34 C33 C31 120.48(19) .
C34 C33 H33 119.8 .
C31 C33 H33 119.8 .
C35 C34 C33 120.1(2) .
C35 C34 H34 120.0 .
C33 C34 H34 120.0 .
C36 C35 C34 119.92(18) .
C36 C35 H35 120.0 .
C34 C35 H35 120.0 .
C35 C36 C32 120.28(19) .
C35 C36 H36 119.9 .
C32 C36 H36 119.9 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N18 1.9548(15) .
Cu1 N11 1.9826(17) .
Cu1 O21 1.9882(14) .
Cu1 Cl1 2.2418(5) .
Cu1 Cl1 2.6143(6) 2_766
Cl1 Cu1 2.6143(6) 2_766
N11 C12 1.345(2) .
N11 C16 1.355(2) .
C12 C13 1.381(3) .
C12 H12 0.9300 .
C13 C14 1.388(3) .
C13 H13 0.9300 .
C14 C15 1.379(3) .
C14 H14 0.9300 .
C15 C16 1.391(3) .
C15 H15 0.9300 .
C16 N17 1.402(2) .
N17 N18 1.298(2) .
N18 C19 1.336(2) .
C19 C20 1.438(3) .
C19 C31 1.476(3) .
C20 O21 1.268(2) .
C20 C41 1.479(3) .
C41 C46 1.391(3) .
C41 C42 1.397(3) .
C42 C43 1.384(3) .
C42 H42 0.9300 .
C43 C44 1.385(3) .
C43 H43 0.9300 .
C44 C45 1.381(3) .
C44 H44 0.9300 .
C45 C46 1.382(3) .
C45 H45 0.9300 .
C46 H46 0.9300 .
C31 C32 1.395(3) .
C31 C33 1.395(3) .
C32 C36 1.393(3) .
C32 H32 0.9300 .
C33 C34 1.388(3) .
C33 H33 0.9300 .
C34 C35 1.389(3) .
C34 H34 0.9300 .
C35 C36 1.381(3) .
C35 H35 0.9300 .
C36 H36 0.9300 .
