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_2017842
_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          '[Mn (C3 H5 N1 O1)6] (Cl O4)2'
_chemical_formula_moiety         'C18 H30 Mn N6 O6 2+, 2(Cl O4 -)'
_chemical_formula_sum            'C18 H30 Cl2 Mn N6 O14'
_chemical_formula_weight         680.32
_chemical_name_systematic
;
Hexakis(prop-2-enamide)manganese(II) bis(perchlorate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.642(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.2804(6)
_cell_length_b                   15.9533(10)
_cell_length_c                   10.6876(7)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.38
_cell_measurement_theta_min      2.42
_cell_volume                     1470.79(17)
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            43193
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.92
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  0.7565
_exptl_absorpt_correction_T_min  0.6616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             702
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.58
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.521
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         5063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0455P)^2^+0.2932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                4083
_reflns_number_total             5063
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gt3024.cif
_cod_data_source_block           II
_cod_original_cell_volume        1470.79(16)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               2017842
_cod_database_fobs_code          2017842