#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/25/7012509.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_7012509
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 H22.5 Cu N3 O5.75'
_chemical_formula_weight         472.46
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 121.990(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.825(3)
_cell_length_b                   5.2237(7)
_cell_length_c                   20.459(3)
_cell_measurement_reflns_used    1956
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      23.8
_cell_measurement_theta_min      2.35
_cell_volume                     2068.9(5)
_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      223(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            5569
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    1.098
_exptl_absorpt_correction_T_max  0.9412
_exptl_absorpt_correction_T_min  0.6352
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'rectangular shape, cut'
_exptl_crystal_F_000             978
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         2767
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0531
_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)+(0.1070P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1673
_reflns_number_gt                2475
_reflns_number_total             2767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211496h.txt
_cod_data_source_block           compound_1
_cod_original_sg_symbol_H-M      Cc
_cod_original_formula_sum        'C21 H22.50 Cu N3 O5.75'
_cod_database_code               7012509
loop_
_symmetry_equiv_pos_as_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'
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 0.40277(4) 0.32422(15) 0.20799(4) 0.0398(3) Uani 1 1 d . . .
O1 O 0.4135(3) 0.3810(15) 0.1223(4) 0.067(2) Uani 1 1 d . . .
O2 O 0.3293(3) 0.5924(10) 0.2004(4) 0.0564(17) Uani 1 1 d . . .
O3 O 0.2173(4) 0.6164(15) 0.1554(6) 0.098(3) Uani 1 1 d . . .
N1 N 0.3194(3) 0.1051(12) 0.1472(4) 0.0462(17) Uani 1 1 d . . .
H1 H 0.3250 -0.0316 0.1784 0.055 Uiso 1 1 calc R . .
N2 N 0.4301(3) 0.1868(12) 0.3155(4) 0.0412(15) Uani 1 1 d . . .
N3 N 0.4841(3) 0.5516(14) 0.2733(4) 0.0455(16) Uani 1 1 d . . .
C1 C 0.3631(6) 0.3760(18) 0.0502(6) 0.056(2) Uani 1 1 d . . .
C2 C 0.3606(7) 0.555(2) -0.0036(7) 0.073(3) Uani 1 1 d . . .
H2 H 0.3963 0.6763 0.0134 0.087 Uiso 1 1 calc R . .
C3 C 0.3078(7) 0.556(2) -0.0794(7) 0.071(3) Uani 1 1 d . . .
H3 H 0.3075 0.6778 -0.1134 0.086 Uiso 1 1 calc R . .
C4 C 0.2567(7) 0.385(3) -0.1052(8) 0.082(4) Uani 1 1 d . . .
H4 H 0.2209 0.3839 -0.1573 0.099 Uiso 1 1 calc R . .
C5 C 0.2572(6) 0.208(2) -0.0539(6) 0.067(3) Uani 1 1 d . . .
H5 H 0.2211 0.0877 -0.0722 0.081 Uiso 1 1 calc R . .
C6 C 0.3085(5) 0.2036(16) 0.0221(6) 0.049(2) Uani 1 1 d . . .
C7 C 0.3122(5) -0.0034(16) 0.0776(5) 0.049(2) Uani 1 1 d . . .
H7A H 0.2702 -0.1078 0.0511 0.059 Uiso 1 1 calc R . .
H7B H 0.3517 -0.1159 0.0921 0.059 Uiso 1 1 calc R . .
C8 C 0.2555(5) 0.2442(18) 0.1323(7) 0.062(3) Uani 1 1 d . . .
H8A H 0.2232 0.2584 0.0765 0.074 Uiso 1 1 calc R . .
H8B H 0.2330 0.1416 0.1530 0.074 Uiso 1 1 calc R . .
C9 C 0.2690(5) 0.5071(16) 0.1669(5) 0.051(2) Uani 1 1 d . . .
C10 C 0.4046(5) 0.0033(17) 0.3379(5) 0.051(2) Uani 1 1 d . . .
H10 H 0.3681 -0.0953 0.2995 0.061 Uiso 1 1 calc R . .
C11 C 0.4280(5) -0.0526(18) 0.4133(6) 0.057(2) Uani 1 1 d . . .
H11 H 0.4069 -0.1842 0.4250 0.069 Uiso 1 1 calc R . .
C12 C 0.4807(4) 0.0795(18) 0.4704(5) 0.051(2) Uani 1 1 d . . .
H12 H 0.4969 0.0402 0.5221 0.061 Uiso 1 1 calc R . .
C13 C 0.5119(5) 0.2797(18) 0.4520(5) 0.050(2) Uani 1 1 d . . .
C14 C 0.5685(4) 0.433(2) 0.5087(5) 0.051(2) Uani 1 1 d . . .
H14 H 0.5866 0.4064 0.5615 0.061 Uiso 1 1 calc R . .
C15 C 0.5953(4) 0.616(2) 0.4856(5) 0.055(2) Uani 1 1 d . . .
H15 H 0.6325 0.7143 0.5232 0.066 Uiso 1 1 calc R . .
C16 C 0.5696(4) 0.6667(15) 0.4066(5) 0.046(2) Uani 1 1 d . . .
C17 C 0.5944(4) 0.8539(17) 0.3793(5) 0.053(2) Uani 1 1 d . . .
H17 H 0.6318 0.9572 0.4142 0.064 Uiso 1 1 calc R . .
C18 C 0.5646(4) 0.8878(18) 0.3024(6) 0.056(2) Uani 1 1 d . . .
H18 H 0.5813 1.0158 0.2841 0.067 Uiso 1 1 calc R . .
C19 C 0.5090(5) 0.7333(18) 0.2497(6) 0.050(2) Uani 1 1 d . . .
H19 H 0.4890 0.7598 0.1965 0.061 Uiso 1 1 calc R . .
C20 C 0.5143(4) 0.5136(15) 0.3508(4) 0.0407(17) Uani 1 1 d . . .
C21 C 0.4841(4) 0.3228(14) 0.3737(5) 0.0371(19) Uani 1 1 d . . .
O1S O 0.0475(9) -0.185(4) 0.1607(10) 0.086(5) Uiso 0.50 1 d P . .
O2S O 0.0267(8) -0.302(3) 0.1348(9) 0.074(4) Uiso 0.50 1 d P . .
O3S O 0.1310(9) -0.581(4) 0.1763(10) 0.081(5) Uiso 0.50 1 d P . .
O4S O 0.1141(10) -0.716(5) 0.1842(11) 0.094(5) Uiso 0.50 1 d P . .
O5S O 0.1485(9) -0.069(4) 0.2228(10) 0.081(4) Uiso 0.50 1 d P . .
O6S O 0.2453(18) 0.008(8) 0.264(2) 0.093(10) Uiso 0.25 1 d 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'
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'
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
O1 Cu1 N1 93.5(3) . . ?
O1 Cu1 N3 89.8(3) . . ?
N1 Cu1 N3 176.3(3) . . ?
O1 Cu1 N2 155.8(3) . . ?
N1 Cu1 N2 96.6(3) . . ?
N3 Cu1 N2 81.2(3) . . ?
O1 Cu1 O2 108.0(3) . . ?
N1 Cu1 O2 83.0(3) . . ?
N3 Cu1 O2 94.3(3) . . ?
N2 Cu1 O2 95.1(3) . . ?
C1 O1 Cu1 124.4(6) . . ?
C9 O2 Cu1 113.7(5) . . ?
C7 N1 C8 113.1(7) . . ?
C7 N1 Cu1 114.1(6) . . ?
C8 N1 Cu1 110.5(5) . . ?
C10 N2 C21 115.6(7) . . ?
C10 N2 Cu1 132.8(6) . . ?
C21 N2 Cu1 111.6(6) . . ?
C19 N3 C20 118.6(7) . . ?
C19 N3 Cu1 127.4(6) . . ?
C20 N3 Cu1 114.0(6) . . ?
O1 C1 C6 122.8(9) . . ?
O1 C1 C2 120.7(10) . . ?
C6 C1 C2 116.5(10) . . ?
C3 C2 C1 121.9(11) . . ?
C4 C3 C2 120.3(10) . . ?
C3 C4 C5 119.3(12) . . ?
C6 C5 C4 121.8(12) . . ?
C5 C6 C1 120.1(10) . . ?
C5 C6 C7 122.1(9) . . ?
C1 C6 C7 117.5(8) . . ?
N1 C7 C6 112.4(7) . . ?
C9 C8 N1 114.2(7) . . ?
O3 C9 O2 127.7(8) . . ?
O3 C9 C8 113.7(8) . . ?
O2 C9 C8 118.5(7) . . ?
N2 C10 C11 124.4(9) . . ?
C12 C11 C10 120.4(9) . . ?
C11 C12 C13 119.4(9) . . ?
C21 C13 C12 115.9(9) . . ?
C21 C13 C14 120.2(9) . . ?
C12 C13 C14 123.9(9) . . ?
C15 C14 C13 119.6(9) . . ?
C14 C15 C16 122.6(8) . . ?
C17 C16 C20 117.0(8) . . ?
C17 C16 C15 125.3(8) . . ?
C20 C16 C15 117.7(8) . . ?
C18 C17 C16 119.9(8) . . ?
C17 C18 C19 120.6(9) . . ?
N3 C19 C18 121.3(9) . . ?
N3 C20 C16 122.5(8) . . ?
N3 C20 C21 116.7(7) . . ?
C16 C20 C21 120.7(7) . . ?
N2 C21 C13 124.4(8) . . ?
N2 C21 C20 116.4(7) . . ?
C13 C21 C20 119.1(7) . . ?
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 O1 1.919(6) . ?
Cu1 N1 1.992(6) . ?
Cu1 N3 2.004(6) . ?
Cu1 N2 2.071(7) . ?
Cu1 O2 2.127(6) . ?
O1 C1 1.304(12) . ?
O2 C9 1.249(11) . ?
O3 C9 1.217(12) . ?
N1 C7 1.459(11) . ?
N1 C8 1.510(12) . ?
N2 C10 1.322(11) . ?
N2 C21 1.375(10) . ?
N3 C19 1.321(12) . ?
N3 C20 1.369(10) . ?
C1 C6 1.391(14) . ?
C1 C2 1.424(15) . ?
C2 C3 1.370(16) . ?
C3 C4 1.336(19) . ?
C4 C5 1.396(19) . ?
C5 C6 1.363(14) . ?
C6 C7 1.538(13) . ?
C8 C9 1.501(12) . ?
C10 C11 1.371(13) . ?
C11 C12 1.342(13) . ?
C12 C13 1.423(14) . ?
C13 C21 1.394(13) . ?
C13 C14 1.439(14) . ?
C14 C15 1.349(15) . ?
C15 C16 1.422(14) . ?
C16 C17 1.386(13) . ?
C16 C20 1.418(11) . ?
C17 C18 1.356(14) . ?
C18 C19 1.405(13) . ?
C20 C21 1.423(12) . ?
O1S O2S 0.79(2) . ?
O3S O4S 0.86(2) . ?
