Constrained ferromagnetic coupling in dinuclear μ1,3-azido nickel(II) cryptate compounds. Crystal structure and magnetic behaviour of [Ni2(L1)(N3)(H2O)][CF3SO3]3·2H2O·EtOH {L1 = N[(CH2)2NHCH2(C6H4-m)CH2NH(CH2)2]3N} †
Escuer, Albert; Harding, Charles J.; Dussart, Yann; Nelson, Jane; McKee, Vickie; Vicente, Ramon; Journal of the Chemical Society, Dalton Transactions  (1999) 223–; doi:10.1039/a806174b

data_7027047
_publ_section_title
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 Constrained ferromagnetic coupling in dinuclear \m1,3-azido nickel(II)
 cryptate compounds. Crystal structure and magnetic behaviour of
 [Ni2(L1)(N3)(H2O)][CF3SO3]3&#x00B7;2H2O&#x00B7;EtOH
 {L1&#x2005;=&#x2005;N[(CH2)2NHCH2(C6H4-m)CH2NH(CH2)2]3N}&#x200A;&#x2020;
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_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              223
_journal_paper_doi               10.1039/a806174b
_journal_year                    1999
_chemical_formula_sum            'C41 H66 F9 N11 Ni2 O13 S3'
_chemical_formula_weight         1305.65
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.3410(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5006(3)
_cell_length_b                   21.0205(4)
_cell_length_c                   16.4021(3)
_cell_measurement_reflns_used    6022
_cell_measurement_temperature    161(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     5453.26(18)
_computing_cell_refinement       SAINT
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXL-97 and SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      161(2)
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with 0.3 degree frames'
_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  0.1078
_diffrn_reflns_av_sigmaI/netI    0.0822
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27832
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.38
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  0.9311
_exptl_absorpt_correction_T_min  0.6807
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         8939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_gt           0.0753
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+30.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1774
_reflns_number_gt                6786
_reflns_number_total             8939
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            806174Bsup1.cif
_cod_data_source_block           nir3bm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+30.0000P] 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^)+(0.0350P)^2^+30.0000P] 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        5453.26(17)
_cod_original_sg_symbol_H-M      'P 2(1)/c'
_cod_database_code               7027047