Crystal structure of <i>trans</i>-diaqua(3,10-dimethyl-1,3,5,8,10,12-hexaazacyclotetradecane)copper(II) pamoate
Tsymbal, Liudmyla V.; Andriichuk, Irina L.; Arion, Vladimir B.; Lampeka, Yaroslaw D.; Acta Crystallographica Section E 75 (2019) 533–536; doi:10.1107/S2056989019003852

data_2242885
_publ_section_title
;
 Crystal structure of
 <i>trans</i>-diaqua(3,10-dimethyl-1,3,5,8,10,12-hexaazacyclotetradecane)copper(II)
 pamoate
;
_journal_coeditor_code           HB7810
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              533
_journal_page_last               536
_journal_paper_doi               10.1107/S2056989019003852
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Cu (C10 H26 N6) (H2 O1)2] C23 H14 O6'
_chemical_formula_moiety         'C10 H30 Cu N6 O2 2+, C23 H14 O6 2-'
_chemical_formula_sum            'C33 H44 Cu N6 O8'
_chemical_formula_weight         716.28
_chemical_name_systematic
;<i>trans</i>-Diaqua(3,10-dimethyl-1,3,5,8,10,12-hexaazacyclotetradecane-\k^4^<i>N</i>^1^,<i>N</i>^5^,<i>N</i>^8^,<i>N</i>^12^)copper(II)
4,4'-methylenebis(3-hydroxynaphthalene-2-carboxylate)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                71.594(3)
_cell_angle_beta                 81.128(3)
_cell_angle_gamma                88.249(3)
_cell_formula_units_Z            2
_cell_length_a                   9.8877(6)
_cell_length_b                   12.1406(7)
_cell_length_c                   14.5760(9)
_cell_measurement_reflns_used    8230
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.642
_cell_measurement_theta_min      2.370
_cell_volume                     1640.06(17)
_computing_cell_refinement
;
SAINT (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            52866
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.920
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.9178
_exptl_absorpt_correction_T_min  0.8682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2007)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             754
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         6401
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.6293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                4540
_reflns_number_total             6401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7810sup1.cif
_cod_data_source_block           I
_cod_database_code               2242885
_cod_database_fobs_code          2242885
_shelx_estimated_absorpt_t_min   0.868
_shelx_estimated_absorpt_t_max   0.918
_shelx_hkl_checksum              47046
_shelx_res_checksum              8681
_shelxl_version_number           2.014