<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>',<i>N</i>''-Pentamethyl-<i>N</i>''-[3-(trimethylazaniumyl)propyl]guanidinium bis(tetraphenylborate)
Tiritiris, Ioannis; Acta Crystallographica Section E 69 (2013) o292–; doi:10.1107/S1600536813001992

data_2237439
_publ_section_title
;
 <i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>',<i>N</i>''-Pentamethyl-<i>N</i>''-[3-(trimethylazaniumyl)propyl]guanidinium
 bis(tetraphenylborate)
;
_journal_coeditor_code           ZL2530
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o292
_journal_paper_doi               10.1107/S1600536813001992
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C12 H30 N4 +, 2C24 H20 B -'
_chemical_formula_moiety         'C12 H30 N4 +, 2C24 H20 B -'
_chemical_formula_sum            'C60 H70 B2 N4'
_chemical_formula_weight         868.82
_chemical_melting_point          502
_chemical_name_systematic
'<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>',<i>N</i>''-Pentamethyl-<i>N</i>''-[3-(trimethylazaniumyl)propyl]guanidinium bis(tetraphenylborate)'
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.0450(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7622(4)
_cell_length_b                   16.1667(3)
_cell_length_c                   17.3787(4)
_cell_measurement_reflns_used    11929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      0.41
_cell_volume                     4941.29(18)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 2004)'
_computing_data_reduction        'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       '\f scans, and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22713
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.16
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         12056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0389P)^2^+2.0808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1078
_reflns_number_gt                8821
_reflns_number_total             12056
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zl2530.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2237439
_cod_database_fobs_code          2237439