#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/10/2241097.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2241097
loop_
_publ_author_name
'Buvaylo, Elena A.'
'Vassilyeva, Olga Yu.'
'Skelton, Brian W.'
_publ_section_title
;
 Crystal structure of
 tetrakis(μ₃-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]:
 a redetermination at 200K
;
_journal_coeditor_code           SJ5474
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1203
_journal_page_last               1206
_journal_paper_doi               10.1107/S2056989015017314
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Cu4 (C12 H15 N O5)4 (H2 O)4]'
_chemical_formula_moiety         'C48 H68 Cu4 N4 O24'
_chemical_formula_sum            'C48 H68 Cu4 N4 O24'
_chemical_formula_weight         1339.22
_chemical_name_systematic
Tetrakis(μ₃-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7108(3)
_cell_length_b                   18.7108(3)
_cell_length_c                   15.3800(3)
_cell_measurement_reflns_used    7964
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.845
_cell_measurement_theta_min      2.748
_cell_volume                     5384.45(16)
_computing_cell_refinement
;
CrysAlis CCD (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis CCD (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis CCD (Agilent, 2013)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR92 (Altomare et al., 1994)
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25330
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         2.771
_exptl_absorpt_coefficient_mu    1.647
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(CrysAlis CCD and CrysAlis RED; Agilent, 2013)
;
_exptl_crystal_colour            dark_green
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       prism
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.58
_refine_diff_density_min         -0.978
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3247
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0763
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0811P)²+52.6317P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1905
_refine_ls_wR_factor_ref         0.1951
_reflns_number_gt                2942
_reflns_number_total             3247
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sj5474sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        5384.4(2)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               2241097
_cod_database_fobs_code          2241097
#BEGIN Tags that were not found in dictionaries:
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Cu Cu1 0.47922(3) 0.66025(3) 0.69100(4) 0.0279(2) Uani d 1
C C1 0.5392(3) 0.5347(3) 0.7698(3) 0.0355(11) Uani d 1
O O1 0.5448(2) 0.58332(19) 0.7095(2) 0.0350(8) Uani d 1
C C2 0.4880(3) 0.5355(3) 0.8386(4) 0.0384(12) Uani d 1
C C3 0.4858(4) 0.4778(4) 0.8971(4) 0.0533(16) Uani d 1
H H3 0.4506 0.4777 0.9416 0.064 Uiso calc 1
C C4 0.5322(5) 0.4225(4) 0.8922(5) 0.063(2) Uani d 1
H H4 0.5285 0.3839 0.9322 0.076 Uiso calc 1
C C5 0.5845(5) 0.4218(3) 0.8297(5) 0.062(2) Uani d 1
H H5 0.6179 0.3836 0.8277 0.075 Uiso calc 1
C C6 0.5887(4) 0.4770(3) 0.7690(4) 0.0531(16) Uani d 1
O O6 0.6377(4) 0.4824(3) 0.7043(4) 0.0781(18) Uani d 1
C C61 0.6974(6) 0.4339(5) 0.7031(7) 0.094(3) Uani d 1
H H61A 0.7184 0.4311 0.7614 0.14 Uiso calc 1
H H61B 0.7334 0.4512 0.6619 0.14 Uiso calc 1
H H61C 0.681 0.3863 0.6852 0.14 Uiso calc 1
C C10 0.4376(3) 0.5937(4) 0.8514(4) 0.0453(14) Uani d 1
H H10 0.4063 0.5904 0.8999 0.054 Uiso calc 1
N N10 0.4318(2) 0.6488(3) 0.8033(3) 0.0416(11) Uani d 1
C C101 0.3781(4) 0.7071(4) 0.8247(4) 0.0492(15) Uani d 1
C C11 0.3629(3) 0.7439(3) 0.7393(4) 0.0384(12) Uani d 1
H H11A 0.3232 0.7186 0.7099 0.046 Uiso calc 1
H H11B 0.3468 0.7933 0.7513 0.046 Uiso calc 1
O O11 0.42189(18) 0.7465(2) 0.6827(2) 0.0322(7) Uani d 1
C C12 0.4105(5) 0.7622(4) 0.8871(5) 0.065(2) Uani d 1
H H12A 0.4533 0.7841 0.8601 0.078 Uiso calc 1
H H12B 0.3753 0.8006 0.8984 0.078 Uiso calc 1
O O12 0.4299(3) 0.7293(3) 0.9664(3) 0.0827(18) Uani d 1
H H12 0.4473 0.76 1.0001 0.124 Uiso calc 1
C C13 0.3123(4) 0.6764(4) 0.8649(4) 0.0551(17) Uani d 1
H H13A 0.3232 0.6592 0.9243 0.066 Uiso calc 1
H H13B 0.2751 0.7139 0.8694 0.066 Uiso calc 1
O O13 0.2862(3) 0.6191(3) 0.8141(4) 0.0724(16) Uani d 1
H H13 0.2492 0.6023 0.8374 0.109 Uiso calc 1
O O2 0.3560(3) 0.5887(2) 0.6505(3) 0.0497(10) Uani d 1
H H2AO 0.341(4) 0.618(4) 0.605(3) 0.075 Uiso d 1
H H2BO 0.326(4) 0.601(4) 0.699(3) 0.075 Uiso d 1
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 0 '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 0.006 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 3 -2 0.0376
-1 -1 0 0.1764
0 -1 -1 0.1086
-3 5 -2 0.0428
0 -1 1 0.0945
4 -2 -3 0.0974
-1 0 2 0.0763
1 0 -1 0.0843
1 0 2 0.0886
-1 0 -2 0.0788
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Cu1 O11 . . 171.70(15)
O1 Cu1 N10 . . 94.41(17)
O11 Cu1 N10 . . 84.16(17)
N10 Cu1 O2 . . 76.41(16)
O11 Cu1 O2 . . 85.77(14)
O1 Cu1 O2 . . 101.89(14)
O1 Cu1 O11 . 16_656 94.54(15)
O11 Cu1 O11 . 16_656 88.41(16)
N10 Cu1 O11 . 16_656 166.34(18)
O2 Cu1 O11 . 2_665 159.30(12)
O1 Cu1 O11 . 16_656 94.54(15)
O11 Cu1 O11 . 16_656 88.44(16)
O1 Cu1 O11 . 2_665 93.29(13)
N10 Cu1 O11 . 2_665 116.70(16)
O11 Cu1 O11 . 2_665 80.15(13)
O11 Cu1 O11 16_656 2_665 73.02(12)
O2 Cu1 O11 . 16_656 91.64(15)
O2 Cu1 O11 . 2_665 159.32(12)
O1 C1 C6 . . 118.1(5)
O1 C1 C2 . . 125.1(5)
C6 C1 C2 . . 116.8(5)
C1 O1 Cu1 . . 125.5(3)
C3 C2 C1 . . 119.2(6)
C3 C2 C10 . . 118.0(6)
C1 C2 C10 . . 122.9(5)
C4 C3 C2 . . 122.2(7)
C4 C3 H3 . . 118.9
C2 C3 H3 . . 118.9
C3 C4 C5 . . 120.2(6)
C3 C4 H4 . . 119.9
C5 C4 H4 . . 119.9
C4 C5 C6 . . 120.2(7)
C4 C5 H5 . . 119.9
C6 C5 H5 . . 119.9
O6 C6 C5 . . 125.7(6)
O6 C6 C1 . . 113.0(5)
C5 C6 C1 . . 121.3(7)
C6 O6 C61 . . 119.2(6)
O6 C61 H61A . . 109.5
O6 C61 H61B . . 109.5
H61A C61 H61B . . 109.5
O6 C61 H61C . . 109.5
H61A C61 H61C . . 109.5
H61B C61 H61C . . 109.5
N10 C10 C2 . . 125.6(5)
N10 C10 H10 . . 117.2
C2 C10 H10 . . 117.2
C10 N10 C101 . . 120.8(5)
C10 N10 Cu1 . . 124.3(4)
C101 N10 Cu1 . . 114.4(3)
C13 C101 C11 . . 112.3(6)
C13 C101 N10 . . 111.0(5)
C11 C101 N10 . . 105.3(4)
C13 C101 C12 . . 109.1(6)
C11 C101 C12 . . 108.2(6)
N10 C101 C12 . . 110.9(5)
O11 C11 C101 . . 113.9(5)
O11 C11 H11A . . 108.8
C101 C11 H11A . . 108.8
O11 C11 H11B . . 108.8
C101 C11 H11B . . 108.8
H11A C11 H11B . . 107.7
C11 O11 Cu1 . . 111.4(3)
C11 O11 Cu1 . 15_566 121.3(3)
Cu1 O11 Cu1 . 15_566 108.47(17)
O12 C12 C101 . . 110.4(6)
O12 C12 H12A . . 109.6
C101 C12 H12A . . 109.6
O12 C12 H12B . . 109.6
C101 C12 H12B . . 109.6
H12A C12 H12B . . 108.1
C12 O12 H12 . . 109.5
O13 C13 C101 . . 110.4(5)
O13 C13 H13A . . 109.6
C101 C13 H13A . . 109.6
O13 C13 H13B . . 109.6
C101 C13 H13B . . 109.6
H13A C13 H13B . . 108.1
C13 O13 H13 . . 109.5
H2AO O2 H2BO . . 105(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 O1 . 1.912(4) y
Cu1 O11 . 1.941(4) y
Cu1 N10 . 1.953(5) y
Cu1 O2 . 2.738(5) y
Cu1 O11 16_656 1.968(3) y
Cu1 O11 2_665 2.547(4) y
C1 O1 . 1.303(6) ?
C1 C6 . 1.422(8) ?
C1 C2 . 1.427(8) ?
C2 C3 . 1.406(8) ?
C2 C10 . 1.455(9) ?
C3 C4 . 1.353(11) ?
C3 H3 . 0.95 ?
C4 C5 . 1.373(11) ?
C4 H4 . 0.95 ?
C5 C6 . 1.394(9) ?
C5 H5 . 0.95 ?
C6 O6 . 1.356(9) ?
O6 C61 . 1.439(9) ?
C61 H61A . 0.98 ?
C61 H61B . 0.98 ?
C61 H61C . 0.98 ?
C10 N10 . 1.273(7) ?
C10 H10 . 0.95 ?
N10 C101 . 1.519(7) ?
C101 C13 . 1.494(9) ?
C101 C11 . 1.510(8) ?
C101 C12 . 1.533(11) ?
C11 O11 . 1.407(6) ?
C11 H11A . 0.99 ?
C11 H11B . 0.99 ?
O11 Cu1 15_566 1.968(3) ?
C12 O12 . 1.414(9) ?
C12 H12A . 0.99 ?
C12 H12B . 0.99 ?
O12 H12 . 0.84 ?
C13 O13 . 1.413(9) ?
C13 H13A . 0.99 ?
C13 H13B . 0.99 ?
O13 H13 . 0.84 ?
O2 H2AO . 0.93(5) ?
O2 H2BO . 0.96(5) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O12 H12 O12 2_665 0.84 2.37 2.736(12) 107.4
O13 H13 O2 3 0.84 1.91 2.700(6) 155.8
O2 H2AO O1 15_566 0.93(5) 1.92(4) 2.791(6) 155(8)
O2 H2AO O6 15_566 0.93(5) 2.23(7) 2.853(7) 124(6)
O2 H2BO O13 . 0.96(5) 1.95(3) 2.892(7) 165(6)
