Crystal structure of bis-{μ<sub>2</sub>-2,2'-[(4,10-dimethyl-1,4,7,10-tetra-aza-cyclo-dodecane-1,7-di-yl)bis(meth-yl-ene)]bis-(4-oxo-4<i>H</i>-pyran-3-olato)}dicobalt-calcium bis-(perchlorate) 1.36-hydrate.
Rossi, Patrizia; Macedi, Eleonora; Paoli, Paola; Giorgi, Luca; Formica, Mauro; Fusi, Vieri; Acta crystallographica. Section E, Crystallographic communications 73 (2017) 1959–1965; doi:10.1107/S2056989017016693

data_2311545
_publ_section_title
;
 Crystal structure of
 bis-{\m<sub>2</sub>-2,2'-[(4,10-dimethyl-1,4,7,10-tetra-aza-cyclo-dodecane-1,7-di-yl)bis(meth-yl-ene)]bis-(4-oxo-4<i>H</i>-pyran-3-olato)}dicobalt-calcium
 bis-(perchlorate) 1.36-hydrate.
;
_journal_coeditor_code           XI2003
_journal_issue                   'Pt 12'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              1959
_journal_page_last               1965
_journal_paper_doi               10.1107/S2056989017016693
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac
'[Ca Co2 (C22 H30 N4 O6)2] (Cl O4)2, 1.36H2 O1'
_chemical_formula_moiety
'C44 H60 Ca Co2 N8 O12 2+, 2(Cl O4 -), 1.36(H2 O1)'
_chemical_formula_sum            'C44 H60 Ca Cl2 Co2 N8 O21.36'
_chemical_formula_weight         1271.92
_chemical_name_systematic
;Bis{\m~2~-2,2'-[(4,10-dimethyl-1,4,7,10-tetraazacyclododecane-1,7-diyl)bis(methylene)]bis(4-oxo-4<i>H</i>-pyran-3-olato)}dicobaltcalcium
bis(perchlorate) 1.36-hydrate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9799(4)
_cell_length_b                   8.9799(4)
_cell_length_c                   32.555(3)
_cell_measurement_reflns_used    1087
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.7982
_cell_measurement_theta_min      3.7354
_cell_volume                     2625.2(3)
_computing_cell_refinement
;
CrysAlis CCD (Oxford Diffraction, 2008)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2008)
;
_computing_data_reduction
;
CrysAlis CCD (Oxford Diffraction, 2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2014 (Burla <i>et al.</i>,  2015)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            3291
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.958
_diffrn_reflns_theta_min         3.755
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2008)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       prism
_exptl_crystal_F_000             1318
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.247
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.14(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.858
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2340
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0355P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                1386
_reflns_number_total             2340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xi2003sup1.cif
_cod_data_source_block           I
_cod_database_code               2311545
_shelx_hkl_checksum              88580
_shelx_res_checksum              99240