Crystal structures of <i>trans</i>-diaqua(3-<i>R</i>-1,3,5,8,12-pentaazacyclotetradecane)copper(II) isophthalate hydrates (<i>R</i> = benzyl or pyridin-3-ylmethyl)
Andriichuk, Irina L.; Tsymbal, Liudmyla V.; Arion, Vladimir B.; Lampeka, Yaroslaw D.; Acta Crystallographica Section E 75 (2019) 1015–1019; doi:10.1107/S2056989019008387

data_2242991
_publ_section_title
;
 Crystal structures of
 <i>trans</i>-diaqua(3-<i>R</i>-1,3,5,8,12-pentaazacyclotetradecane)copper(II)
 isophthalate hydrates (<i>R</i> = benzyl or pyridin-3-ylmethyl)
;
_journal_coeditor_code           HB7828
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1015
_journal_page_last               1019
_journal_paper_doi               10.1107/S2056989019008387
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac
'[Cu (C15 H28 N6) (H2 O)2] (C8 H4 O4), 0.9H2 O'
_chemical_formula_moiety         'C15 H32 Cu N6 O2 2+, C8 H4 O4 2-, 0.9(H2 O)'
_chemical_formula_sum            'C23 H37.8 Cu N6 O6.9'
_chemical_formula_weight         572.33
_chemical_name_systematic
;<i>trans</i>-Diaqua[3-(pyridin-3-ylmethyl)-1,3,5,8,12-pentaazacyclotetradecane-\k^4^<i>N</i>^1^,<i>N</i>^5^,<i>N</i>^8^,<i>N</i>^12^]copper(II)
isophthalate 0.9-hydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 94.276(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1955(3)
_cell_length_b                   19.0463(8)
_cell_length_c                   19.4426(8)
_cell_measurement_reflns_used    6756
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.124
_cell_measurement_theta_min      3.453
_cell_volume                     2657.15(19)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1057
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            76082
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.741
_diffrn_reflns_theta_min         2.357
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_T_max  0.9659
_exptl_absorpt_correction_T_min  0.8727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2007)
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       needle
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.337
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         4532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+2.3396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                2834
_reflns_number_total             4532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7828sup1.cif
_cod_data_source_block           II
_cod_original_formula_sum        'C23 H37.80 Cu N6 O6.90'
_cod_database_code               2242991
_shelx_estimated_absorpt_t_min   0.873
_shelx_estimated_absorpt_t_max   0.966
_shelx_hkl_checksum              21741
_shelx_res_checksum              91874
_shelxl_version_number           2.014
_cod_database_fobs_code 2242991