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_7043721
_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 O2'
_chemical_formula_sum            'C22 H28 Fe O2'
_chemical_formula_weight         380.29
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-01-22 deposited with the CCDC.
2017-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.019(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2649(3)
_cell_length_b                   16.7822(6)
_cell_length_c                   15.3281(7)
_cell_measurement_reflns_used    2498
_cell_measurement_temperature    270(2)
_cell_measurement_theta_max      66.804
_cell_measurement_theta_min      3.917
_cell_volume                     1834.36(13)
_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_publication_material  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_diffrn_ambient_temperature      270(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra, Ruby CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8530
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.202
_diffrn_reflns_theta_max         67.202
_diffrn_reflns_theta_min         3.946
_exptl_absorpt_coefficient_mu    6.674
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.61253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       needle
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.114
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0730
_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^)+(0.0550P)^2^+6.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.1803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2646
_reflns_number_total             3255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02037f2.cif
_cod_data_source_block           gk442
_cod_database_code               7043721
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.181
_shelx_estimated_absorpt_t_max   0.776
_shelx_res_checksum              26994