Structure and isomerization comparison of Zn(ii), Cd(ii) and Hg(ii) perchlorate complexes of 2,6-bis([(2-pyridyl-methyl)amino]methyl)pyridine.
Carra, Bradley J.; Berry, Steven M.; Pike, Robert D.; Bebout, Deborah C.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 14424–14431; doi:10.1039/c3dt51741a

data_7021961
_publ_section_title
;
 Structure and isomerization comparison of Zn(ii), Cd(ii) and Hg(ii)
 perchlorate complexes of
 2,6-bis([(2-pyridyl-methyl)amino]methyl)pyridine.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14424
_journal_page_last               14431
_journal_paper_doi               10.1039/c3dt51741a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C19 H21 Cd Cl2 N5 O8'
_chemical_formula_sum            'C19 H21 Cd Cl2 N5 O8'
_chemical_formula_weight         630.71
_chemical_name_common
diperchlorato-(2,6-bis([(2-pyridylmethyl)amino]methyl)pyridine)-cadmium(ii)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                74.250(2)
_cell_angle_beta                 81.541(2)
_cell_angle_gamma                65.904(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1253(3)
_cell_length_b                   9.1478(3)
_cell_length_c                   15.9271(5)
_cell_measurement_reflns_used    6939
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      72.04
_cell_measurement_theta_min      2.89
_cell_volume                     1167.12(7)
_computing_cell_refinement       'SAINTPLUS (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2004)'
_computing_data_reduction        SAINTPLUS
_computing_molecular_graphics    'SHELXLE (Hubschle, 2011)'
_computing_publication_material  'Mercury 3.1 (CCDC, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.864
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\w and \y'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.864
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19926
_diffrn_reflns_point_group_measured_fraction_full 0.864
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         62.489
_diffrn_reflns_theta_min         2.885
_exptl_absorpt_coefficient_mu    10.110
_exptl_absorpt_correction_T_max  0.1952
_exptl_absorpt_correction_T_min  0.0950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         3643
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0499P)^2^+1.0004P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3532
_reflns_number_total             3643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt51741a.txt
_cod_data_source_block           Compound2
_cod_database_code               7021961
_shelx_estimated_absorpt_t_min   0.095
_shelx_estimated_absorpt_t_max   0.195
_shelxl_version_number           2013-2
_shelx_res_checksum              90128
_shelx_hkl_checksum              99385