Axial chiral metallocenes by two-fold ring-closing metathesis.
Buchowicz, W.; Furmańczyk, A; Zachara, J.; Majchrzak, M.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 9269–9271; doi:10.1039/c2dt31291c

data_7019933
_publ_section_title
;
 Axial chiral metallocenes by two-fold ring-closing metathesis.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9269
_journal_page_last               9271
_journal_paper_doi               10.1039/c2dt31291c
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C30 H42 Fe'
_chemical_formula_sum            'C30 H42 Fe'
_chemical_formula_weight         458.49
_chemical_name_systematic
;
?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-01-17
_audit_creation_method
;
Olex2 1.1
(compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                67.653(2)
_cell_angle_beta                 86.4663(18)
_cell_angle_gamma                75.074(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8147(2)
_cell_length_b                   10.9245(3)
_cell_length_c                   13.1469(3)
_cell_measurement_reflns_used    33325
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      30.4196
_cell_measurement_theta_min      3.2043
_cell_volume                     1258.73(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.3347
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_details
;
1 omega -86.00 -19.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -13.6182 148.0000 -144.0000 67

2 omega -84.00 -50.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -13.6182 146.0000 60.0000 34

3 omega -16.00 92.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 13.9307 77.0000 -120.0000 108

4 omega -12.00 88.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 13.9307 38.0000 -180.0000 100

5 omega -60.00 28.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 13.9307 -39.0000 119.0000 88

6 omega -35.00 48.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 13.9307 -77.0000 -120.0000 83

7 omega -63.00 48.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 13.9307 -77.0000 60.0000 111

8 omega -18.00 89.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 13.9307 77.0000 30.0000 107

9 omega -88.00 -13.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -13.6182 151.0000 166.0000 75

10 omega -103.00 -32.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -13.6182 179.0000 -60.0000 71

11 omega -40.00 62.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -13.6182 38.0000 -180.0000 102

12 omega -12.00 90.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 13.9307 38.0000 -150.0000 102

13 omega -12.00 90.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 13.9307 38.0000 -30.0000 102

14 omega -13.00 90.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 13.9307 39.0000 93.0000 103

15 omega -88.00 -13.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -13.6182 151.0000 -69.0000 75

16 omega -75.00 -1.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -13.6182 131.0000 -7.0000 74

17 omega -92.00 20.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -13.6182 -77.0000 -120.0000 112

18 omega -40.00 62.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -13.6182 38.0000 -60.0000 102

19 omega -83.00 -10.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -13.6182 145.0000 137.0000 73

20 omega 56.00 104.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 13.9307 179.0000 -120.0000 48

21 omega -103.00 -32.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -13.6182 179.0000 120.0000 71

22 omega -84.00 -10.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -13.6182 146.0000 60.0000 74

23 omega -92.00 -17.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -13.6182 157.0000 -26.0000 75

24 omega -103.00 74.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- -13.6182 0.0000 -180.0000 177

25 omega 56.00 104.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 13.9307 179.0000 30.0000 48
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0657441000
_diffrn_orient_matrix_UB_12      0.0164169000
_diffrn_orient_matrix_UB_13      -0.0279571000
_diffrn_orient_matrix_UB_21      0.0202144000
_diffrn_orient_matrix_UB_22      -0.0626403000
_diffrn_orient_matrix_UB_23      -0.0082337000
_diffrn_orient_matrix_UB_31      -0.0295354000
_diffrn_orient_matrix_UB_32      -0.0327643000
_diffrn_orient_matrix_UB_33      0.0505858000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            75409
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         30.49
_diffrn_reflns_theta_min         3.21
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           40
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.166
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7236
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.7080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                6294
_reflns_number_total             7236
_reflns_threshold_expression     I>2u(I)
_cod_data_source_file            c2dt31291c.txt
_cod_data_source_block           b_f16
_cod_original_cell_volume        1258.72(5)
_cod_database_code               7019933