Cyclopentadienide Ligand CpC‒ Possessing Intrinsic Helical Chirality and Its Ferrocene Analogues
Chung, Jae-Yeon; Schulz, Christian; Bauer, Heiko; Sun, Yu; Sitzmann, Helmut; Auerbach, Hendrik; Pierik, Antonio J.; Schünemann, Volker; Neuba, Adam; Thiel, Werner R.; Organometallics 34 (2015) 5374–; doi:10.1021/acs.organomet.5b00673

data_4087879
_publ_section_title
;
 Cyclopentadienide Ligand CpC-- Possessing Intrinsic Helical Chirality and
 Its Ferrocene Analogues
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5374
_journal_paper_doi               10.1021/acs.organomet.5b00673
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C49 H52 B Cl2 F4 Fe'
_chemical_formula_weight         854.46
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.379(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2995(3)
_cell_length_b                   21.6161(5)
_cell_length_c                   14.5263(3)
_cell_measurement_reflns_used    5057
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.4640
_cell_measurement_theta_min      3.0810
_cell_volume                     4172.47(16)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Giacovazzo et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1399
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27887
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.524
_diffrn_reflns_theta_min         2.774
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       plate
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.541
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.077
_refine_diff_density_max         1.571
_refine_diff_density_min         -1.190
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         13669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+6.3198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9906
_reflns_number_total             13669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00673_si_005.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4087879
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.758
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              17612
_shelx_hkl_checksum              3157