Syntheses, Structures, and Magnetic Characterization of Dicyanometalate(II) Building Blocks: [NEt4][(Tp*)MII(CN)2] [MII = Cr, Co, Ni; Tp* = hydridotris(3,5-diemethylpyrazolyl)borate]
Stephen Holmes; Rodolphe Clerac; Dongfeng Li.; Sean Parkin; Chad Ruschman; Chemical Communications  (2006) –; doi:10.1039/b608297a

data_7101438
_publ_section_title
;
Syntheses, Structures, and Magnetic Characterization
of Dicyanometalate(II) Building Blocks: [NEt4][(Tp*)MII(CN)2] [MII = Cr,
Co, Ni; Tp* = hydridotris(3,5-diemethylpyrazolyl)borate]
;
_journal_issue                   38
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b608297a
_journal_year                    2006
_chemical_formula_sum            'C28 H48.5 B Cr N9.5 O0.5'
_chemical_formula_weight         589.07
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.565(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1192(3)
_cell_length_b                   13.9716(4)
_cell_length_c                   24.4089(7)
_cell_measurement_reflns_used    6076
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      67.63
_cell_measurement_theta_min      3.62
_cell_volume                     3449.68(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker X8 Proteum CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0908
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40970
_diffrn_reflns_theta_full        68.10
_diffrn_reflns_theta_max         68.10
_diffrn_reflns_theta_min         4.37
_exptl_absorpt_coefficient_mu    2.978
_exptl_absorpt_correction_T_max  0.9293
_exptl_absorpt_correction_T_min  0.5873
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            purple-orange
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         6213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0761
_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^)+(0.1309P)^2^+5.9795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2104
_refine_ls_wR_factor_ref         0.2234
_reflns_number_gt                4925
_reflns_number_total             6213
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b608297a.txt
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C28 H48.50 B Cr N9.50 O0.50'
_cod_database_code               7101438