Crystal structures of 1'-aminocobaltocenium-1-carboxylic acid chloride monohydrate and of its azo dye 1'-[2-(1-amino-2,6-dimethylphenyl)diazen-1-yl]cobaltocenium-1-carboxylic acid hexafluoridophosphate monohydrate
Jochriem, Markus; Wurst, Klaus; Kopacka, Holger; Bildstein, Benno; Acta Crystallographica Section E 75 (2019) 208–213; doi:10.1107/S2056989019000562

data_2242809
_publ_section_title
;
 Crystal structures of 1'-aminocobaltocenium-1-carboxylic acid chloride
 monohydrate and of its azo dye
 1'-[2-(1-amino-2,6-dimethylphenyl)diazen-1-yl]cobaltocenium-1-carboxylic
 acid hexafluoridophosphate monohydrate
;
_journal_coeditor_code           WM5478
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              208
_journal_page_last               213
_journal_paper_doi               10.1107/S2056989019000562
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Co (C5 H6 N) (C6 H5 O2)] Cl, H2 O'
_chemical_formula_moiety         'C11 H11 Co N O2 +, Cl -, H2 O'
_chemical_formula_sum            'C11 H13 Cl Co N O3'
_chemical_formula_weight         301.60
_chemical_name_systematic
;
1'-Aminocobaltocenium-1-carboxylic acid chloride monohydrate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7269(5)
_cell_length_b                   6.7024(3)
_cell_length_c                   11.7607(4)
_cell_measurement_reflns_used    9295
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      50.7
_cell_measurement_theta_min      2.7
_cell_volume                     1160.85(8)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX3 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
<i>CHEMDRAW</i> (Cambridge Soft, 2001) and
ORTEP-3 for Windows (Farrugia,
2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi layered optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14289
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.715
_diffrn_reflns_theta_min         2.766
_diffrn_source                   'Incoatec Microfocus'
_exptl_absorpt_coefficient_mu    1.702
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_description       plate
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.312
_refine_ls_abs_structure_details
;
 Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.067(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2163
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+0.1150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0455
_refine_ls_wR_factor_ref         0.0459
_reflns_number_gt                2099
_reflns_number_total             2163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5478sup1.cif
_cod_data_source_block           3
_cod_database_code               2242809
_shelx_estimated_absorpt_t_min   0.809
_shelx_estimated_absorpt_t_max   0.951
_shelx_hkl_checksum              13047
_shelx_res_checksum              52283
_cod_database_fobs_code 2242809