Crystal structures of bis[(9<i>S</i>,13<i>S</i>,14<i>S</i>)-3-methoxy-17-methylmorphinanium] tetrachloridocobaltate and tetrachloridocuprate
Gauchat, Eric; Nazarenko, Alexander Y.; Acta Crystallographica Section E 73 (2017) 63–67; doi:10.1107/S2056989016019939

data_2241988
_publ_section_title
;
 Crystal structures of
 bis[(9<i>S</i>,13<i>S</i>,14<i>S</i>)-3-methoxy-17-methylmorphinanium]
 tetrachloridocobaltate and tetrachloridocuprate
;
_journal_coeditor_code           SJ5517
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              63
_journal_page_last               67
_journal_paper_doi               10.1107/S2056989016019939
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '(C18 H26 N O)2 [Co Cl4]'
_chemical_formula_moiety         '2(C18 H26 N O +), Cl4 Co 2-'
_chemical_formula_sum            'C36 H52 Cl4 Co N2 O2'
_chemical_formula_weight         745.52
_chemical_name_systematic
;
Bis[(9<i>S</i>,13<i>S</i>,14<i>S</i>)-3-methoxy-17-methylmorphinanium]
tetrachloridocobaltate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.605(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8447(6)
_cell_length_b                   9.2316(4)
_cell_length_c                   14.7018(6)
_cell_measurement_reflns_used    9174
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.89
_cell_volume                     1852.68(14)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015)
;
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker PHOTON-100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            43153
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.772
_diffrn_reflns_theta_min         2.810
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_T_max  0.9785
_exptl_absorpt_correction_T_min  0.7610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS, Bruker, 2015)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       plate
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.483
_exptl_crystal_size_mid          0.262
_exptl_crystal_size_min          0.141
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.257
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1711 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack   0.000(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         4803
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0494P)^2^+0.4319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                4183
_reflns_number_total             4803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj5517sup1.cif
_cod_data_source_block           a
_cod_database_code               2241988
_shelx_estimated_absorpt_t_min   0.703
_shelx_estimated_absorpt_t_max   0.897
_shelx_hkl_checksum              65107
_shelx_res_checksum              9493
_cod_database_fobs_code 2241988