Crystal structure of tetrakis(μ~3~-2-{[1,1-bis(hydroxymethyl)-2-oxidoethyl]iminomethyl}-6-methoxyphenolato)tetrakis[aquacopper(II)]: a redetermination at 200K
Buvaylo, Elena A.; Vassilyeva, Olga Yu.; Skelton, Brian W.; Acta Crystallographica Section E 71 (2015) 1203–1206; doi:10.1107/S2056989015017314

data_2241097
_publ_section_title
;
 Crystal structure of
 tetrakis(\m~3~-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(\m~3~-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
;
<i>CrysAlis CCD</i> (Agilent, 2013)
;
_computing_data_collection
;
<i>CrysAlis CCD</i> (Agilent, 2013)
;
_computing_data_reduction
;
<i>CrysAlis CCD</i> (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 <i>et al.</i>, 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       '\w 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
;
(<i>CrysAlis CCD</i> and <i>CrysAlis RED</i>; 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/[\s^2^(Fo^2^)+(0.0811P)^2^+52.6317P] where P=(Fo^2^+2Fc^2^)/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>2\s(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
_shelx_hkl_checksum              24139
_shelx_res_checksum              47253