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_7043722
_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         'C22 H28 Fe O'
_chemical_formula_sum            'C22 H28 Fe O'
_chemical_formula_weight         364.29
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-03-18T20:54:27-00:00
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.3755(9)
_cell_length_b                   15.528(2)
_cell_length_c                   20.3832(17)
_cell_measurement_reflns_used    2252
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.969
_cell_measurement_theta_min      4.333
_cell_volume                     3600.5(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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 0.982
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0812499
_diffrn_orient_matrix_UB_12      -0.025665
_diffrn_orient_matrix_UB_13      0.0572618
_diffrn_orient_matrix_UB_21      -0.0350979
_diffrn_orient_matrix_UB_22      0.095245
_diffrn_orient_matrix_UB_23      0.0094848
_diffrn_orient_matrix_UB_31      -0.1024349
_diffrn_orient_matrix_UB_32      -0.0117877
_diffrn_orient_matrix_UB_33      -0.0483038
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_unetI/netI     0.0913
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.98
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10036
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.98
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.814
_diffrn_reflns_theta_min         5.286
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.732
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.412
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
      CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.94
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0629
_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^)+(0.0873P)^2^+5.5896P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1628
_refine_ls_wR_factor_ref         0.1854
_reflns_number_gt                2359
_reflns_number_total             3201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02037f2.cif
_cod_data_source_block           gk423
_cod_database_code               7043722
_shelx_res_checksum              26693