#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/25/7012510.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_7012510
loop_
_publ_author_name
'Yang, Chang-Tong'
'Moubaraki, Boujemaa'
'Murray, Keith S.'
'Vittal, Jagadese J.'
_publ_section_title
;
 Synthesis, characterization and properties of ternary copper(ii)
 complexes containing reduced Schiff base N-(2-hydroxybenzyl)-α-amino
 acids and 1,10-phenanthrolineElectronic supplementary information
 (ESI) available: ESI-MS and UV titration data. See
 http://www.rsc.org/suppdata/dt/b2/b211496h/
;
_journal_issue                   5
_journal_name_full               'Dalton Transactions'
_journal_page_first              880
_journal_paper_doi               10.1039/b211496h
_journal_year                    2003
_chemical_formula_sum            'C21 H21 Cl Cu N3 O8.5'
_chemical_formula_weight         550.40
_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
_cell_angle_alpha                96.4630(10)
_cell_angle_beta                 95.9790(10)
_cell_angle_gamma                93.2340(10)
_cell_formula_units_Z            2
_cell_length_a                   7.8954(5)
_cell_length_b                   9.7201(6)
_cell_length_c                   14.9638(9)
_cell_measurement_reflns_used    4510
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.06
_cell_volume                     1132.18(12)
_computing_cell_refinement       'Bruker AXS, SAINT'
_computing_data_collection       'Bruker AXS, SMART'
_computing_data_reduction        'Bruker AXS, SAINT'
_computing_molecular_graphics    'Bruker AXS, SHELXTL'
_computing_publication_material  'Bruker AXS, SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      253(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_method       'ω scans'
_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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11075
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_T_max  0.9186
_exptl_absorpt_correction_T_min  0.8133
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'rhombohedral blocks'
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.294
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         3993
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.243
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1220P)²+0.2604P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1667
_refine_ls_wR_factor_ref         0.1735
_reflns_number_gt                3380
_reflns_number_total             3993
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211496h.txt
_cod_data_source_block           compound_4
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C21 H21 Cl Cu N3 O8.50'
_cod_database_code               7012510
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.24324(7) 0.02211(5) 0.18044(4) 0.0408(3) Uani 1 1 d . . .
O1 O 0.0389(6) 0.2021(4) 0.1808(3) 0.0526(10) Uani 1 1 d . . .
H1A H 0.058(11) 0.240(8) 0.157(5) 0.08(3) Uiso 1 1 d . . .
C1 C 0.0590(6) 0.2619(5) 0.2694(3) 0.0467(11) Uani 1 1 d . . .
C2 C 0.1152(7) 0.4002(5) 0.2938(4) 0.0562(13) Uani 1 1 d . . .
H2 H 0.1358 0.4578 0.2499 0.067 Uiso 1 1 calc R . .
C3 C 0.1401(9) 0.4509(6) 0.3851(4) 0.0704(17) Uani 1 1 d . . .
H3 H 0.1775 0.5434 0.4024 0.084 Uiso 1 1 calc R . .
C4 C 0.1106(9) 0.3672(6) 0.4495(4) 0.0699(17) Uani 1 1 d . . .
H4 H 0.1257 0.4033 0.5103 0.084 Uiso 1 1 calc R . .
C5 C 0.0585(8) 0.2291(6) 0.4253(4) 0.0629(14) Uani 1 1 d . . .
H5 H 0.0408 0.1720 0.4698 0.075 Uiso 1 1 calc R . .
C6 C 0.0319(6) 0.1741(5) 0.3335(3) 0.0460(11) Uani 1 1 d . . .
C7 C -0.0168(7) 0.0232(5) 0.3062(4) 0.0547(13) Uani 1 1 d . . .
H7A H -0.0637 -0.0161 0.3559 0.066 Uiso 1 1 calc R . .
H7B H -0.1047 0.0125 0.2550 0.066 Uiso 1 1 calc R . .
N1 N 0.1317(5) -0.0533(4) 0.2813(3) 0.0428(9) Uani 1 1 d . . .
H1 H 0.200(7) -0.060(5) 0.333(4) 0.048(14) Uiso 1 1 d . . .
C8 C 0.0827(7) -0.2029(5) 0.2501(4) 0.0532(13) Uani 1 1 d . . .
H8A1 H -0.0250 -0.2290 0.2716 0.064 Uiso 1 1 calc R . .
H8B1 H 0.1687 -0.2593 0.2754 0.064 Uiso 1 1 calc R . .
C9 C 0.0656(6) -0.2300(5) 0.1481(3) 0.0443(11) Uani 1 1 d . . .
O2 O 0.1179(5) -0.1328(3) 0.1054(2) 0.0526(9) Uani 1 1 d . . .
O3 O 0.0018(5) -0.3442(3) 0.1118(3) 0.0613(10) Uani 1 1 d . . .
N2 N 0.4199(5) 0.1630(4) 0.2497(3) 0.0407(9) Uani 1 1 d . . .
C10 C 0.4633(6) 0.1942(5) 0.3380(3) 0.0494(12) Uani 1 1 d . . .
H10 H 0.4126 0.1411 0.3772 0.059 Uiso 1 1 calc R . .
C11 C 0.5814(7) 0.3028(5) 0.3745(4) 0.0561(13) Uani 1 1 d . . .
H11 H 0.6087 0.3213 0.4368 0.067 Uiso 1 1 calc R . .
C12 C 0.6562(7) 0.3815(5) 0.3181(4) 0.0567(13) Uani 1 1 d . . .
H12 H 0.7342 0.4551 0.3418 0.068 Uiso 1 1 calc R . .
C13 C 0.6160(6) 0.3518(5) 0.2244(4) 0.0468(11) Uani 1 1 d . . .
C14 C 0.4960(5) 0.2414(4) 0.1935(3) 0.0395(10) Uani 1 1 d . . .
C15 C 0.4484(5) 0.2050(4) 0.0981(3) 0.0389(10) Uani 1 1 d . . .
C16 C 0.5218(6) 0.2802(5) 0.0357(3) 0.0464(11) Uani 1 1 d . . .
C17 C 0.4694(7) 0.2372(6) -0.0560(4) 0.0554(13) Uani 1 1 d . . .
H17 H 0.5144 0.2830 -0.1004 0.066 Uiso 1 1 calc R . .
C18 C 0.3515(7) 0.1274(6) -0.0794(4) 0.0567(14) Uani 1 1 d . . .
H18 H 0.3164 0.0984 -0.1402 0.068 Uiso 1 1 calc R . .
C19 C 0.2837(6) 0.0591(5) -0.0138(3) 0.0487(11) Uani 1 1 d . . .
H19 H 0.2025 -0.0147 -0.0312 0.058 Uiso 1 1 calc R . .
N3 N 0.3323(5) 0.0968(4) 0.0741(3) 0.0407(9) Uani 1 1 d . . .
C20 C 0.6859(7) 0.4291(6) 0.1589(4) 0.0574(13) Uani 1 1 d . . .
H20 H 0.7630 0.5050 0.1786 0.069 Uiso 1 1 calc R . .
C21 C 0.6425(7) 0.3943(5) 0.0701(4) 0.0557(13) Uani 1 1 d . . .
H21 H 0.6921 0.4456 0.0296 0.067 Uiso 1 1 calc R . .
Cl1 Cl 0.5549(2) -0.22293(18) 0.34113(13) 0.0817(5) Uani 1 1 d D . .
O4 O 0.5366(18) -0.1167(13) 0.2849(8) 0.120(2) Uiso 0.50 1 d PD A .
O5 O 0.7192(13) -0.2451(14) 0.3685(9) 0.120(2) Uiso 0.50 1 d PD A .
O6 O 0.4609(15) -0.3462(11) 0.2864(8) 0.120(2) Uiso 0.50 1 d PD A .
O7 O 0.4447(15) -0.1839(13) 0.4092(8) 0.120(2) Uiso 0.50 1 d PD A .
O4A O 0.7198(14) -0.2834(13) 0.3216(9) 0.119(2) Uiso 0.50 1 d PD A 1
O5A O 0.4642(15) -0.3077(12) 0.3840(8) 0.119(2) Uiso 0.50 1 d PD A 1
O6A O 0.6332(15) -0.1058(11) 0.4138(8) 0.119(2) Uiso 0.50 1 d PD A 1
O7A O 0.4912(19) -0.1553(14) 0.2706(8) 0.119(2) Uiso 0.50 1 d PD A 1
O8 O -0.1096(6) -0.3839(4) -0.0707(3) 0.0606(10) Uani 1 1 d D . .
H8A H -0.063(7) -0.354(6) -0.0139(17) 0.071(12) Uiso 1 1 d D . .
H8B H -0.072(7) -0.468(3) -0.084(4) 0.071(12) Uiso 1 1 d D . .
O9 O 0.2735(11) -0.0459(10) 0.4727(6) 0.072(2) Uani 0.50 1 d PD . .
H9A H 0.262(13) -0.1391(12) 0.467(9) 0.071(12) Uiso 0.50 1 d PD . .
H9B H 0.172(7) -0.018(9) 0.451(8) 0.071(12) Uiso 0.50 1 d PD . .
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'
Cl Cl 0.1484 0.1585 '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'
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
_geom_angle_publ_flag
O2 Cu1 N3 92.39(15) . . ?
O2 Cu1 N1 84.39(15) . . ?
N3 Cu1 N1 174.66(15) . . ?
O2 Cu1 N2 167.17(16) . . ?
N3 Cu1 N2 82.43(15) . . ?
N1 Cu1 N2 101.58(16) . . ?
O1 C1 C6 116.1(4) . . ?
O1 C1 C2 122.2(5) . . ?
C6 C1 C2 121.5(5) . . ?
C1 C2 C3 118.6(5) . . ?
C4 C3 C2 120.9(5) . . ?
C3 C4 C5 120.4(5) . . ?
C4 C5 C6 120.3(6) . . ?
C1 C6 C5 118.2(5) . . ?
C1 C6 C7 120.8(4) . . ?
C5 C6 C7 120.9(5) . . ?
N1 C7 C6 111.5(4) . . ?
C7 N1 C8 111.9(4) . . ?
C7 N1 Cu1 113.0(3) . . ?
C8 N1 Cu1 106.2(3) . . ?
N1 C8 C9 110.8(4) . . ?
O3 C9 O2 124.4(5) . . ?
O3 C9 C8 118.2(4) . . ?
O2 C9 C8 117.4(4) . . ?
C9 O2 Cu1 114.8(3) . . ?
C10 N2 C14 117.7(4) . . ?
C10 N2 Cu1 130.8(3) . . ?
C14 N2 Cu1 111.5(3) . . ?
N2 C10 C11 122.9(5) . . ?
C12 C11 C10 119.3(5) . . ?
C11 C12 C13 120.0(5) . . ?
C14 C13 C12 117.0(4) . . ?
C14 C13 C20 118.4(5) . . ?
C12 C13 C20 124.6(4) . . ?
N2 C14 C13 123.2(4) . . ?
N2 C14 C15 116.8(4) . . ?
C13 C14 C15 120.1(4) . . ?
N3 C15 C16 123.4(4) . . ?
N3 C15 C14 116.3(4) . . ?
C16 C15 C14 120.3(4) . . ?
C17 C16 C15 116.6(4) . . ?
C17 C16 C21 125.4(5) . . ?
C15 C16 C21 117.9(5) . . ?
C18 C17 C16 119.3(5) . . ?
C17 C18 C19 120.7(5) . . ?
N3 C19 C18 121.4(5) . . ?
C19 N3 C15 118.6(4) . . ?
C19 N3 Cu1 128.6(3) . . ?
C15 N3 Cu1 112.7(3) . . ?
C21 C20 C13 121.4(5) . . ?
C20 C21 C16 121.9(5) . . ?
O5A Cl1 O5 104.2(8) . . ?
O5A Cl1 O7A 125.2(8) . . ?
O5 Cl1 O7A 129.1(9) . . ?
O5A Cl1 O4 141.5(8) . . ?
O5 Cl1 O4 114.1(7) . . ?
O7A Cl1 O4 21.4(8) . . ?
O5A Cl1 O7 53.2(7) . . ?
O5 Cl1 O7 118.2(7) . . ?
O7A Cl1 O7 102.2(9) . . ?
O4 Cl1 O7 102.2(7) . . ?
O5A Cl1 O6 62.5(7) . . ?
O5 Cl1 O6 112.9(7) . . ?
O7A Cl1 O6 83.3(7) . . ?
O4 Cl1 O6 103.9(7) . . ?
O7 Cl1 O6 103.8(6) . . ?
O5A Cl1 O4A 110.4(7) . . ?
O5 Cl1 O4A 30.2(6) . . ?
O7A Cl1 O4A 110.4(9) . . ?
O4 Cl1 O4A 104.9(8) . . ?
O7 Cl1 O4A 146.1(7) . . ?
O6 Cl1 O4A 89.1(7) . . ?
O5A Cl1 O6A 105.7(7) . . ?
O5 Cl1 O6A 69.6(7) . . ?
O7A Cl1 O6A 104.3(7) . . ?
O4 Cl1 O6A 84.8(7) . . ?
O7 Cl1 O6A 66.0(6) . . ?
O6 Cl1 O6A 168.1(7) . . ?
O4A Cl1 O6A 96.6(6) . . ?
O7A O4 Cl1 75.4(17) . . ?
O4A O5 Cl1 85.6(12) . . ?
O4A O5 O6A 136.7(17) . . ?
Cl1 O5 O6A 60.4(6) . . ?
O5A O6 Cl1 53.3(5) . . ?
O5A O7 Cl1 58.6(6) . . ?
O5A O7 O6A 104.9(9) . . ?
Cl1 O7 O6A 59.9(5) . . ?
O5 O4A Cl1 64.2(10) . . ?
O7 O5A Cl1 68.2(7) . . ?
O7 O5A O6 116.3(10) . . ?
Cl1 O5A O6 64.2(6) . . ?
Cl1 O6A O7 54.1(5) . . ?
Cl1 O6A O5 50.1(4) . . ?
O7 O6A O5 94.0(7) . . ?
O4 O7A Cl1 83.2(18) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.931(3) . ?
Cu1 N3 1.998(4) . ?
Cu1 N1 2.011(4) . ?
Cu1 N2 2.015(4) . ?
O1 C1 1.376(6) . ?
C1 C6 1.378(7) . ?
C1 C2 1.388(7) . ?
C2 C3 1.390(8) . ?
C3 C4 1.359(9) . ?
C4 C5 1.378(8) . ?
C5 C6 1.407(7) . ?
C6 C7 1.495(7) . ?
C7 N1 1.481(7) . ?
N1 C8 1.493(6) . ?
C8 C9 1.510(7) . ?
C9 O3 1.235(6) . ?
C9 O2 1.273(6) . ?
N2 C10 1.326(6) . ?
N2 C14 1.360(6) . ?
C10 C11 1.391(7) . ?
C11 C12 1.358(8) . ?
C12 C13 1.399(8) . ?
C13 C14 1.395(6) . ?
C13 C20 1.435(7) . ?
C14 C15 1.435(6) . ?
C15 N3 1.347(6) . ?
C15 C16 1.401(6) . ?
C16 C17 1.399(8) . ?
C16 C21 1.433(7) . ?
C17 C18 1.365(8) . ?
C18 C19 1.381(7) . ?
C19 N3 1.334(6) . ?
C20 C21 1.337(8) . ?
Cl1 O5A 1.324(10) . ?
Cl1 O5 1.356(9) . ?
Cl1 O7A 1.372(10) . ?
Cl1 O4 1.408(10) . ?
Cl1 O7 1.439(10) . ?
Cl1 O6 1.486(10) . ?
Cl1 O4A 1.501(10) . ?
Cl1 O6A 1.537(10) . ?
O4 O7A 0.52(2) . ?
O5 O4A 0.757(15) . ?
O5 O6A 1.657(16) . ?
O6 O5A 1.464(16) . ?
O7 O5A 1.242(15) . ?
O7 O6A 1.623(16) . ?
