Structural and Magnetic Diversity in Tetraalkylammonium Salts of Anionic M[N(CN)2]3- (M= Mn and Ni) Three-Dimensional Coordination Polymers
John A. Schlueter; Jamie L. Manson; Urs Geiser; Inorganic Chemistry 44 (2005) 3194–3202; doi:10.1021/ic0484598

data_4308822
_publ_section_title
;
Structural and Magnetic Diversity in Tetraalkylammonium Salts of
Anionic M[N(CN)2]3- (M= Mn and Ni) Three-Dimensional Coordination Polymers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3194
_journal_page_last               3202
_journal_paper_doi               10.1021/ic0484598
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         '(C16 H36 N, Ni, C6 N9)'
_chemical_formula_sum            'C22 H36 N10 Ni'
_chemical_formula_weight         499.32
_chemical_melting_point          468
_chemical_name_common
;
Tetrabutylammonium nickel(II) dicyanamide
;
_chemical_name_systematic
; 
Tetrabutylammonium nickel(II) dicyanamide
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.6842(5)
_cell_length_b                   15.6841(6)
_cell_length_c                   21.1551(8)
_cell_measurement_reflns_used    1877
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.520
_cell_measurement_theta_min      2.597
_cell_volume                     5204.0(3)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Siemens SMART CCD area detector'
_diffrn_measurement_method       'area detector \w 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  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42356
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  0.891
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(Sheldrick, 2001)
;
_exptl_crystal_colour            'greenish blue'
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         12186
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.7336P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.1025
_reflns_number_gt                8000
_reflns_number_total             12186
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0484598si20041103_041216_7.cif
_cod_data_source_block           TBANiDCART
_cod_database_code               4308822