New Reactivity at the Silicon Bridge in Sila[1]ferrocenophanes
Musgrave, Rebecca Alice; Hailes, Rebekah; Schäfer, André; Russell, Andrew David; Gates, Paul Jonathan; Manners, Ian; Dalton Transactions  (2018) –; doi:10.1039/C7DT04593J

data_7045346
_publ_section_title
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 New Reactivity at the Silicon Bridge in Sila[1]ferrocenophanes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT04593J
_journal_year                    2018
_chemical_formula_moiety         'C19 H27 Fe N Si'
_chemical_formula_sum            'C19 H27 Fe N Si'
_chemical_formula_weight         353.3549
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           45
_space_group_name_Hall           'I 2 -2c'
_space_group_name_H-M_alt        'I b a 2'
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-12-05 deposited with the CCDC.
2018-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.6524(4)
_cell_length_b                   27.8481(10)
_cell_length_c                   8.8550(3)
_cell_measurement_reflns_used    5900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.65
_cell_volume                     3366.61(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.03
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14677
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.924
_diffrn_reflns_theta_min         1.462
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0582 before and 0.0470 after correction.
The Ratio of minimum to maximum transmission is 0.8969.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       plate
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.552
_exptl_crystal_size_mid          0.304
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 1423 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3733
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0311P)^2^+0.2274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0592
_reflns_Friedel_coverage         0.735
_reflns_Friedel_fraction_full    0.858
_reflns_Friedel_fraction_max     0.841
_reflns_number_gt                3539
_reflns_number_total             3733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04593j2.cif
_cod_data_source_block           rm422
_cod_original_cell_volume        3366.6(2)
_cod_database_code               7045346
_shelxl_version_number           2014-1
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.02) H3(0.022) H4(0.021) H5(0.018) H7(0.017) H8(0.02)
 H9(0.019) H10(0.017) H12A(0.018) H12B(0.018) H13A(0.019) H13B(0.019)
 H14A(0.018) H14B(0.018) H16A(0.025) H16B(0.025) H16C(0.025) H17A(0.025)
 H17B(0.025) H17C(0.025) H18A(0.022) H18B(0.022) H18C(0.022) H19A(0.022)
 H19B(0.022) H19C(0.022)
 Fixed X: H2(0.3225) H3(0.3431) H4(0.3713) H5(0.3672) H7(0.111) H8(0.0662)
 H9(0.0855) H10(0.1408) H12A(0.4124) H12B(0.3525) H13A(0.2685) H13B(0.2636)
 H14A(0.1735) H14B(0.1149) H16A(0.4418) H16B(0.4928) H16C(0.4118) H17A(0.3335)
 H17B(0.4458) H17C(0.3741) H18A(0.0658) H18B(0.1782) H18C(0.1222) H19A(0.0997)
 H19B(0.0209) H19C(0.0587)
 Fixed Y: H2(0.2157) H3(0.2696) H4(0.2169) H5(0.13) H7(0.1986) H8(0.2477)
 H9(0.195) H10(0.1129) H12A(0.0449) H12B(0.0111) H13A(0.0166) H13B(0.0741)
 H14A(0.0075) H14B(0.0396) H16A(0.0962) H16B(0.0629) H16C(0.0408) H17A(0.1376)
 H17B(0.1291) H17C(0.1568) H18A(0.1208) H18B(0.1352) H18C(0.151) H19A(0.034)
 H19B(0.0524) H19C(0.0877)
 Fixed Z: H2(0.1362) H3(0.3636) H4(0.5947) H5(0.5075) H7(0.1483) H8(0.3792)
 H9(0.6103) H10(0.5229) H12A(-0.2179) H12B(-0.1046) H13A(-0.3365) H13B(-0.3211)
 H14A(-0.1167) H14B(-0.236) H16A(0.1449) H16B(0.0204) H16C(0.1311) H17A(-
 0.1976) H17B(-0.1526) H17C(-0.0392) H18A(-0.1765) H18B(-0.2005) H18C(-0.0497)
 H19A(0.1137) H19B(-0.007) H19C(0.123)
;
_shelx_res_checksum              10092
_olex2_submission_special_instructions 'No special instructions were received'