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_2243534
_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_formula_iupac          '[Fe (C5 H5) (C8 H12 N)]'
_chemical_formula_moiety         'C13 H17 Fe N'
_chemical_formula_sum            'C13 H17 Fe N'
_chemical_formula_weight         243.12
_chemical_name_systematic
;
[(<i>N</i>,<i>N</i>-Dimethylamino)methyl]ferrocene
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
OLEX2
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.590(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.6777(3)
_cell_length_b                   23.0873(15)
_cell_length_c                   8.7206(6)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.13
_cell_measurement_theta_min      2.50
_cell_volume                     1143.06(12)
_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
;
SHELXT (Sheldrick, 2015b)
;
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker D8 VENTURE area detector'
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19466
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.996
_diffrn_reflns_theta_min         2.497
_diffrn_source                   'Advanced Light Source, station 11.3.1'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.284
_exptl_absorpt_correction_T_max  0.4353
_exptl_absorpt_correction_T_min  0.3508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       needle
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.546
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.191
_refine_diff_density_max         1.335
_refine_diff_density_min         -1.471
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         3960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0175P)^2^+3.6060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                3489
_reflns_number_total             3960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7933sup1.cif
_cod_data_source_block           1
_cod_database_code               2243534
_shelx_hkl_checksum              83431
_shelx_res_checksum              53966
_cod_database_fobs_code 2243534