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_4308816
_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, Mn, C6 N9)'
_chemical_formula_sum            'C18 H28 Mn N10'
_chemical_formula_weight         439.44
_chemical_melting_point          525
_chemical_name_common
; 
Tetrapropylammonium manganese (II) dicyanamide
;
_chemical_name_systematic
; 
Tetrapropylammonium manganese (II) dicyanamide
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL-97 cif file'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.2945(4)
_cell_length_b                   16.2945(4)
_cell_length_c                   17.4321(8)
_cell_measurement_reflns_used    1995
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.520
_cell_measurement_theta_min      2.500
_cell_volume                     4628.4(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      298(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44694
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        <1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(Sheldrick, 2001)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.271
_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   0.24(2)
_refine_ls_extinction_coef       0.0229(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         5524
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+1.9779P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                4816
_reflns_number_total             5524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0484598si20041103_041216_1.cif
_cod_data_source_block           TPrAMndcaRT
_cod_database_code               4308816