Crystal structure of <i>N</i>-[3-(dimethylamino)propyl]-<i>N</i>',<i>N</i>',<i>N</i>'',<i>N</i>''-tetramethyl-<i>N</i>-(<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylformamidiniumyl)guanidinium bis(tetraphenylborate)
Tiritiris, Ioannis; Kantlehner, Willi; Acta Crystallographica Section E 71 (2015) o1045–o1046; doi:10.1107/S2056989015023336

data_2241407
_publ_section_title
;
 Crystal structure of
 <i>N</i>-[3-(dimethylamino)propyl]-<i>N</i>',<i>N</i>',<i>N</i>'',<i>N</i>''-tetramethyl-<i>N</i>-(<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylformamidiniumyl)guanidinium
 bis(tetraphenylborate)
;
_journal_coeditor_code           NR2062
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1045
_journal_page_last               o1046
_journal_paper_doi               10.1107/S2056989015023336
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C15 H36 N6 2+, 2C24 H20 B -'
_chemical_formula_moiety         'C15 H36 N6 2+, 2(C24 H20 B -)'
_chemical_formula_sum            'C63 H76 B2 N6'
_chemical_formula_weight         938.92
_chemical_name_systematic
'<i>N</i>-[3-(Dimethylamino)propyl]-<i>N</i>',<i>N</i>',<i>N</i>'',<i>N</i>''-tetramethyl-<i>N</i>-(<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylformamidiniumyl)guanidinium bis(tetraphenylborate)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90.00
_cell_angle_beta                 98.7520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1964(5)
_cell_length_b                   17.6641(7)
_cell_length_c                   17.4751(6)
_cell_measurement_reflns_used    6372
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      0.41
_cell_volume                     5246.4(3)
_computing_cell_refinement
;
DENZO-SMN (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Hooft, 2004)
;
_computing_data_reduction
;
DENZO-SMN (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2005)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0112
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11667
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.199
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 4294 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.8(8)
_refine_ls_extinction_coef       0.0028(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         11660
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+3.2124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0872
_reflns_number_gt                10531
_reflns_number_total             11660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nr2062sup1.cif
_cod_data_source_block           I
_cod_database_code               2241407
_cod_database_fobs_code          2241407
_shelx_hkl_checksum              88298
_shelx_res_checksum              21215