Crystal structures of [(<i>N</i>,<i>N</i>-dimethylamino)methyl]ferrocene and (<i>R</i>~p~,<i>R</i>~p~)-bis{2-[(dimethylamino)methyl]ferrocenyl}dimethylsilane
Krupp, Anna; Wegge, Jessica; Otte, Felix; Kleinheider, Johannes; Wall, Helene; Strohmann, Carsten; Acta Crystallographica Section E 76 (2020) 1437–1441; doi:10.1107/S2056989020010397

data_2243535
_publ_section_title
;
 Crystal structures of [(<i>N</i>,<i>N</i>-dimethylamino)methyl]ferrocene
 and
 (<i>R</i>~p~,<i>R</i>~p~)-bis{2-[(dimethylamino)methyl]ferrocenyl}dimethylsilane
;
_journal_coeditor_code           HB7933
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1437
_journal_page_last               1441
_journal_paper_doi               10.1107/S2056989020010397
_journal_volume                  76
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_iupac          '[Fe2 (C5 H5)2 (C18 H18 N2 Si)]'
_chemical_formula_moiety         'C28 H38 Fe2 N2 Si'
_chemical_formula_sum            'C28 H38 Fe2 N2 Si'
_chemical_formula_weight         542.39
_chemical_name_systematic
(<i>R</i>~p~,<i>R</i>~p~)-Bis{2-[(dimethylamino)methyl]ferrocenyl}dimethylsilane
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;
OLEX2
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0132(7)
_cell_length_b                   14.0683(8)
_cell_length_c                   15.7169(11)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    100
_cell_measurement_theta_max      78.64
_cell_measurement_theta_min      4.22
_cell_volume                     2656.2(3)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009),
publCIF (Westrip, 2010), Mercury
(Macrae <i>et al.</i>,  2020)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015a)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker D8 VENTURE area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'HELIOS mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41156
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.929
_diffrn_reflns_theta_min         4.217
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.315
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.3258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            'clear orangish yellow'
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.474
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.273
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2287 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.009(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0111P)^2^+2.2762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0646
_reflns_number_gt                5518
_reflns_number_total             5733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7933sup1.cif
_cod_data_source_block           2
_cod_database_code               2243535
_shelx_estimated_absorpt_t_min   0.096
_shelx_estimated_absorpt_t_max   0.516
_shelx_hkl_checksum              67397
_shelx_res_checksum              29634
_cod_database_fobs_code 2243535