Bis[(5<i>RS</i>,11<i>RS</i>)-2,8-dimethyl-5,10-methano-5,6,11,12-tetrahydrodibenzo[<i>b</i>,<i>f</i>][1,5]diazocine-5-ium dihydrogen phosphate] tris(phosphoric acid) methanol solvate
Matulková, Irena; Teubner, Karel; Němec, Ivan; Rohovec, Jan; Mička, Zdeněk; Acta Crystallographica Section E 61 (2005) o3941–o3943; doi:10.1107/S1600536805034781

data_2207281
_publ_section_title
;Bis[(5<i>RS</i>,11<i>RS</i>)-2,8-dimethyl-5,10-methano-5,6,11,12-tetrahydrodibenzo[<i>b</i>,<i>f</i>][1,5]diazocine-5-ium
 dihydrogen phosphate] tris(phosphoric acid) methanol solvate
;
_journal_coeditor_code           KP6067
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3941
_journal_page_last               o3943
_journal_paper_doi               10.1107/S1600536805034781
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac
'2C17 H19 N2 + , 2H2 O4 P - , 3H3 O4 P , C H4 O'
_chemical_formula_moiety
'2C17 H19 N2 + , 2H2 O4 P - , 3H3 O4 P , C H4 O'
_chemical_formula_sum            'C35 H55 N4 O21 P5'
_chemical_formula_weight         1022.68
_chemical_name_systematic
;
Bis[(5RS,11RS)-2,8-dimethyl-5,10-methano-5,6,11,12-
tetrahydrodibenzo[b,f][1,5]diazocine-5-ium dihydrogen phosphate]
tris(phosphoric acid) methanol solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                76.9690(13)
_cell_angle_beta                 88.3810(14)
_cell_angle_gamma                88.3660(15)
_cell_formula_units_Z            2
_cell_length_a                   10.1330(2)
_cell_length_b                   10.3690(2)
_cell_length_c                   22.4040(6)
_cell_measurement_reflns_used    10003
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2291.84(9)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'SCALEPACK and DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\w and \f scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0829
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42017
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.80
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.283
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.48200(10)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.457
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         10505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0589P)^2^+0.239P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                6499
_reflns_number_total             10505
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kp6067.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               2207281
_cod_database_fobs_code          2207281