1-D and 2-D Homoleptic Dicyanamide Structures, [Ph4P]2{CoII[N(CN)2]4} and [Ph4P]{M[N(CN)2]3} (M = Mn, Co)
James W. Raebiger; Jamie L. Manson; Roger D. Sommer; Urs Geiser; Arnold L. Rheingold; Joel S. Miller; Inorganic Chemistry 40 (2001) 2578–2581; doi:10.1021/ic001379t

data_4319685
_publ_section_title
;
 1-D and 2-D Homoleptic Dicyanamide Structures, [Ph4P]2{CoII[N(CN)2]4} and
 [Ph4P]{M[N(CN)2]3} (M = Mn, Co)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2578
_journal_page_last               2581
_journal_paper_doi               10.1021/ic001379t
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         (Ph4P){Co[N(CN)2]3}
_chemical_formula_sum            'C30 H20 Co N9 P'
_chemical_formula_weight         596.45
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 101.0870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.4354(10)
_cell_length_b                   7.4426(5)
_cell_length_c                   14.1556(10)
_cell_measurement_reflns_used    3403
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.153
_cell_measurement_theta_min      2.325
_cell_volume                     1389.06(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6965
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.8145
_exptl_absorpt_correction_T_min  0.8145
_exptl_absorpt_correction_type   'Empirical from SADABS'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0299P)^2^+1.2488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1054
_reflns_number_gt                2544
_reflns_number_total             3212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001379t_2.cif
_cod_data_source_block           jsm41
_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 
;
_cod_database_code               4319685