Molecular and Electronic Structures of Bis(pyridine-2,6-diimine)metal Complexes [ML2](PF6)n (n = 0, 1, 2, 3; M = Mn, Fe, Co, Ni, Cu, Zn)
Bas de Bruin; Eckhard Bill; Eberhard Bothe; Thomas Weyhermüller; Karl Wieghardt; Inorganic Chemistry 39 (2000) 2936–2947; doi:10.1021/ic000113j

data_4321074
_publ_section_title
;
 Molecular and Electronic Structures of Bis(pyridine-2,6-diimine)metal
 Complexes [ML2](PF6)n (n = 0, 1, 2, 3; M = Mn, Fe, Co, Ni, Cu, Zn)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2936
_journal_page_last               2947
_journal_paper_doi               10.1021/ic000113j
_journal_volume                  39
_journal_year                    2000
_chemical_formula_structural     '[C46 H46 Fe N6 O4]2+, 2 (P F6)-, H2O'
_chemical_formula_sum            'C46 H48 F12 Fe N6 O5 P2'
_chemical_formula_weight         1110.69
_chemical_name_systematic
; 
 ? 
;
_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           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 114.81(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.455(2)
_cell_length_b                   16.4501(12)
_cell_length_c                   17.224(2)
_cell_measurement_reflns_used    18666
_cell_measurement_temperature    100(2)
_cell_volume                     4746.4(11)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\w, 679 frames a 40 sec.'
_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  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            81673
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_type   'Not measured'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       'opaque block'
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.805
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.121
_refine_ls_goodness_of_fit_obs   1.249
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         13822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_restrained_S_obs      1.249
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_obs          0.0420
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1290
_refine_ls_wR_factor_obs         0.1166
_reflns_number_observed          10052
_reflns_number_total             13832
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000113j_3.cif
_cod_data_source_block           '[Fe(II)L(0)2]2+'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4746.4(8)
_cod_database_code               4321074