9-<i>O</i>-Ethylberberrubinium iodide monohydrate
Grundt, Peter; Pernat, Jennifer; Krivogorsky, Bogdana; Halverson, Melanie A.; Berry, Steven M.; Acta Crystallographica Section E 66 (2010) o2585–o2586; doi:10.1107/S1600536810036664

data_2227736
_publ_section_title
;
 9-<i>O</i>-Ethylberberrubinium iodide monohydrate
;
_journal_coeditor_code           JJ2056
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2585
_journal_page_last               o2586
_journal_paper_doi               10.1107/S1600536810036664
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '2C21 H20 N O4 +, 2I -, H2 O'
_chemical_formula_moiety         '2(C21 H20 N O4 +), 2(I -), H2 O'
_chemical_formula_sum            'C42 H42 I2 N2 O9'
_chemical_formula_weight         972.61
_chemical_melting_point          257
_chemical_name_common
'9-<i>O</i>-Ethylberberrubinium iodide monohydrate'
_chemical_name_systematic
;
9-ethoxy-10-methoxy-5,6-dihydro-1,3-dioxolo[4,5-<i>g</i>]isoquinolino[3,2-\
<i>a</i>]isoquinolin-7-ium iodide monohydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                80.442(6)
_cell_angle_beta                 71.121(5)
_cell_angle_gamma                76.875(5)
_cell_formula_units_Z            2
_cell_length_a                   11.036(3)
_cell_length_b                   13.449(4)
_cell_length_c                   14.086(4)
_cell_measurement_reflns_used    50086
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3
_cell_volume                     1916.8(9)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'CrystalClear (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear (Rigaku, 2009)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>, 1996)'
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_solution
'CrystalStructure (Rigaku, 2009) and SIR2004 (Burla <i>et al.</i>, 2005)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'image plate'
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II image plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Mo sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.101
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            50086
_diffrn_reflns_theta_full        27.484
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.072
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.701
_exptl_absorpt_correction_T_max  0.712
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             972
_exptl_crystal_size_max          1.000
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.75
_refine_diff_density_min         -2.26
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9565
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     502
_refine_ls_number_reflns         8751
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.0006227
_refine_ls_shift/su_mean         0.0000142
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994; Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
4.85 6.23 1.54
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1947
_refine_ls_wR_factor_gt          0.1569
_refine_ls_wR_factor_ref         0.1947
_reflns_number_gt                4563
_reflns_number_total             8751
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            jj2056.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               2227736
_cod_database_fobs_code          2227736