Deltoid versus Rhomboid: Controlling the Shape of Bis-ferrocene Macrocycles by the Bulkiness of the Substituents
Hoffmann, Viktor; le Pleux, Loïc; Häussinger, Daniel; Unke, Oliver T.; Prescimone, Alessandro; Mayor, Marcel; Organometallics 36 (2017) 858–; doi:10.1021/acs.organomet.6b00909

data_4087035
_publ_section_title
;
 Deltoid versus Rhomboid: Controlling the Shape of Bis-ferrocene
 Macrocycles by the Bulkiness of the Substituents
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              858
_journal_paper_doi               10.1021/acs.organomet.6b00909
_journal_volume                  36
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_compound_source        'Viktor Hoffmann'
_chemical_formula_moiety         'C40 H24 Fe2'
_chemical_formula_sum            'C40 H24 Fe2'
_chemical_formula_weight         616.32
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-03
_audit_creation_method           CRYSTALS_ver_14.61
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2693(7)
_cell_length_b                   15.9085(12)
_cell_length_c                   18.2694(14)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    123
_cell_measurement_theta_max      70
_cell_measurement_theta_min      5
_cell_volume                     2694.0(4)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12826
_diffrn_reflns_theta_full        70.138
_diffrn_reflns_theta_max         70.139
_diffrn_reflns_theta_min         3.684
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.851
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_recrystallization_method
; 
DCM 
;
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.23
_refine_ls_abs_structure_details 'Flack (1983), 1911 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.021(5)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8648
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         4571
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.0012310
_refine_ls_shift/su_mean         0.0000552
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 4.79 7.28 3.49 0.877 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0812
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0812
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                3812
_reflns_number_total             4571
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0392
_oxford_refine_ls_scale          0.08066(2)
_oxford_reflns_number_all        4571
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'vh367_123k_0m in P2(1)2(1)2(1)'
_cod_data_source_file            om6b00909_si_005.cif
_cod_data_source_block           vh367_123k
_cod_depositor_comments          'Adding full bibliography for 4087035.cif.'
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               4087035