Triple ring contraction of a [2+2] macrocyclic ligand
Knapton, Matthew; McKee, Vickie; Acta Crystallographica Section C 69 (2013) 837–840; doi:10.1107/S010827011301768X

data_2019077
_publ_section_title
;
 Triple ring contraction of a [2+2] macrocyclic ligand
;
_journal_coeditor_code           EG3130
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              837
_journal_page_last               840
_journal_paper_doi               10.1107/S010827011301768X
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Cu (C2 H3 O2) (C20 H22 N6 O2)] Cl O4'
_chemical_formula_moiety         'C22 H25 Cu N6 O4 +, Cl O4 -'
_chemical_formula_sum            'C22 H25 Cl Cu N6 O8'
_chemical_formula_weight         600.47
_chemical_name_systematic
'(Acetato-\k<i>O</i>)[26,28-dioxa-3,7,15,19,25,27-hexaazahexacyclo[19.3.1.1^2,5^.1^9,13^.1^17,20^.0^3,8^]octacosa-1(25),9(27),10,12,14,21,23-heptaene-\k^5^<i>N</i>]copper(II) perchlorate'
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL2012
_cell_angle_alpha                90
_cell_angle_beta                 103.3500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9252(8)
_cell_length_b                   16.9606(15)
_cell_length_c                   16.5461(14)
_cell_measurement_reflns_used    7293
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.40
_cell_volume                     2437.0(4)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'APEX2 (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_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            24778
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.363
_diffrn_reflns_theta_min         1.744
_exptl_absorpt_coefficient_mu    1.068
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2009)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.270
_refine_diff_density_max         1.531
_refine_diff_density_min         -1.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         6075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0580P)^2^+2.6210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1152
_reflns_number_gt                5050
_reflns_number_total             6075
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3130.cif
_cod_data_source_block           2
_cod_database_code               2019077
_cod_database_fobs_code          2019077
_shelx_estimated_absorpt_t_min   0.693
_shelx_estimated_absorpt_t_max   0.761
_shelx_hkl_checksum              13313
_shelx_res_checksum              75653
_shelxl_version_number           .000002012