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_4308818
_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         '(C12 H28 N, Ni, C6 N9)'
_chemical_formula_sum            'C18 H28 N10 Ni'
_chemical_formula_weight         443.21
_chemical_melting_point          538
_chemical_name_common
; 
Tetrapropylammonium nickel (II) dicyanamide
;
_chemical_name_systematic
; 
Tetrapropylammonium nickel (II) dicyanamide
;
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_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            16
_cell_length_a                   17.1711(15)
_cell_length_b                   22.9918(18)
_cell_length_c                   22.750(2)
_cell_measurement_reflns_used    1008
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.940
_cell_measurement_theta_min      2.911
_cell_volume                     8981.6(13)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            84875
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.889
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(Sheldrick, 2001)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.079
_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     495
_refine_ls_number_reflns         10843
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+24.6118P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1512
_reflns_number_gt                8449
_reflns_number_total             10843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0484598si20041103_041216_3.cif
_cod_data_source_block           TPrANidcaRT
_cod_original_cell_volume        8981.4(13)
_cod_original_formula_sum        'C18 H28 Ni N10'
_cod_database_code               4308818