Control over cyclisation sequences of 1,1’-bifunctional octamethylferrocenes to ferrocenophanes
Roemer, Max; Wild, Duncan Andrew; Skelton, Brian W.; Sobolev, Alexandre N.; Nealon, Gareth; Piggott, Matthew; Koutsantonis, George; Dalton Trans.  (2017) –; doi:10.1039/C7DT02037F

data_7043723
_publ_section_title
;
 Control over cyclisation sequences of 1,1&#x2019;-bifunctional
 octamethylferrocenes to ferrocenophanes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02037F
_journal_year                    2017
_chemical_formula_moiety         'C46 H59 Fe2 N'
_chemical_formula_sum            'C46 H59 Fe2 N'
_chemical_formula_weight         737.64
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-12-19T09:30:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-01-22 deposited with the CCDC.
2017-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.573(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2794(9)
_cell_length_b                   8.5648(7)
_cell_length_c                   25.8751(13)
_cell_measurement_reflns_used    7161
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.638
_cell_measurement_theta_min      2.564
_cell_volume                     3821.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0841894
_diffrn_orient_matrix_UB_12      0.0227987
_diffrn_orient_matrix_UB_13      -0.0221355
_diffrn_orient_matrix_UB_21      -0.0283222
_diffrn_orient_matrix_UB_22      -0.0051809
_diffrn_orient_matrix_UB_23      0.0552786
_diffrn_orient_matrix_UB_31      0.0099109
_diffrn_orient_matrix_UB_32      0.1784215
_diffrn_orient_matrix_UB_33      0.0043958
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.1021
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            35388
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.3
_diffrn_reflns_theta_max         67.3
_diffrn_reflns_theta_min         2.562
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.316
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_correction_T_min  0.318
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)

;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       needle
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.478
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.024
_refine_diff_density_max         1.486
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         6773
_refine_ls_number_restraints     300
_refine_ls_restrained_S_all      1.412
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0829
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1365P)^2^+8.9316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2209
_refine_ls_wR_factor_ref         0.238
_reflns_number_gt                5313
_reflns_number_total             6773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02037f2.cif
_cod_data_source_block           gk442a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7043723
_shelx_res_checksum              44154