Hexakis(prop-2-enamide)copper(II) bis(perchlorate) and hexakis(prop-2-enamide)manganese(II) bis(perchlorate)
Kellett, Andrew; Rosair, Georgina; Devereux, Michael; McNamara, Mary; McCann, Malachy; Acta Crystallographica Section C 66 (2010) m358–m362; doi:10.1107/S0108270110038813

data_2017841
_publ_section_title
;
 Hexakis(prop-2-enamide)copper(II) bis(perchlorate) and
 hexakis(prop-2-enamide)manganese(II) bis(perchlorate)
;
_journal_coeditor_code           GT3024
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m358
_journal_page_last               m362
_journal_paper_doi               10.1107/S0108270110038813
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Cu (C3 H5 N1 O1)6] (Cl O4)2'
_chemical_formula_moiety         'C18 H30 Cu N6 O6 2+ , 2(Cl O4 -)'
_chemical_formula_sum            'C18 H30 Cl2 Cu N6 O14'
_chemical_formula_weight         688.92
_chemical_name_systematic
;
Hexakis(prop-2-enamide)copper(II) bis(perchlorate)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.392(3)
_cell_angle_beta                 85.871(3)
_cell_angle_gamma                83.690(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4577(5)
_cell_length_b                   9.8762(6)
_cell_length_c                   17.7889(11)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.83
_cell_measurement_theta_min      2.30
_cell_volume                     1472.77(15)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34176
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.02
_diffrn_reflns_theta_min         2.08
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  0.7411
_exptl_absorpt_correction_T_min  0.5029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             710
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.576
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         9130
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+0.5550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                7503
_reflns_number_total             9130
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gt3024.cif
_cod_data_source_block           I
_cod_database_code               2017841