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_7019934
_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                67.2990(19)
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_cell_formula_units_Z            2
_cell_length_a                   9.8085(2)
_cell_length_b                   10.9220(2)
_cell_length_c                   13.2038(3)
_cell_measurement_reflns_used    41307
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      31.7022
_cell_measurement_theta_min      3.1904
_cell_volume                     1264.02(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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 0.926
_diffrn_measurement_details
;
1 omega -93.00 -67.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -15.7963 154.0000 58.0000 26

2 omega -76.00 -46.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -15.7963 129.0000 3.0000 30

3 omega -20.00 58.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -15.7963 77.0000 -30.0000 78

4 omega -72.00 -38.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -15.7963 -179.0000 -30.0000 34

5 omega -93.00 -49.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -15.7963 154.0000 -72.0000 44

6 omega -54.00 22.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 -57.0000 -90.0000 76

7 omega -57.00 50.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 -77.0000 -180.0000 107

8 omega 39.00 75.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 38.0000 -30.0000 36

9 omega 56.00 98.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 179.0000 60.0000 42

10 omega -11.00 95.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 77.0000 30.0000 106

11 omega 4.00 95.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 77.0000 -120.0000 91

12 omega 30.00 58.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 -99.0000 60.0000 28

13 omega 17.00 45.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 -69.0000 70.0000 28

14 omega -12.00 90.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 57.0000 -180.0000 102

15 omega 42.00 75.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 18.0000 -124.0000 -56.0000 33

16 omega -92.00 11.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -15.7963 -38.0000 -60.0000 103

17 omega -106.00 -34.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -15.7963 -179.0000 0.0000 72

18 omega -90.00 14.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -15.7963 -57.0000 -150.0000 104

19 omega -106.00 -34.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- -15.7963 -179.0000 -180.0000 72

20 omega 56.00 106.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 179.0000 -180.0000 50

21 omega -10.00 92.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 38.0000 -120.0000 102

22 omega 53.00 105.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 -179.0000 -60.0000 52

23 omega -4.00 58.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 -99.0000 30.0000 62

24 omega -60.00 43.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 -38.0000 -180.0000 103

25 omega -16.00 92.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 69.0000 109.0000 108

26 omega -13.00 90.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 57.0000 -60.0000 103

27 omega 17.00 75.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 18.0000 -124.0000 -56.0000 58

28 omega -10.00 92.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 38.0000 -180.0000 102

29 omega -73.00 106.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 0.0000 -180.0000 179

30 omega -73.00 106.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 0.0000 -150.0000 179

31 omega -73.00 106.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 0.0000 -120.0000 179

32 omega -73.00 106.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 0.0000 -90.0000 179

33 omega -73.00 106.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 0.0000 -60.0000 179

34 omega -73.00 106.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 0.0000 -30.0000 179

35 omega -73.00 -8.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 0.0000 0.0000 65

36 omega 56.00 106.00 1.0000 15.0000
omega____ theta____ kappa____ phi______ frames
- 16.1088 179.0000 -90.0000 50
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0281362000
_diffrn_orient_matrix_UB_12      0.0696909000
_diffrn_orient_matrix_UB_13      -0.0331151000
_diffrn_orient_matrix_UB_21      0.0619450000
_diffrn_orient_matrix_UB_22      0.0009019000
_diffrn_orient_matrix_UB_23      -0.0311617000
_diffrn_orient_matrix_UB_31      -0.0307315000
_diffrn_orient_matrix_UB_32      -0.0199400000
_diffrn_orient_matrix_UB_33      -0.0364105000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            112046
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         31.77
_diffrn_reflns_theta_min         3.20
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           40
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.545
_exptl_crystal_size_mid          0.289
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         7975
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0460P)^2^+0.5416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                6952
_reflns_number_total             7975
_reflns_threshold_expression     I>2u(I)
_cod_data_source_file            c2dt31291c.txt
_cod_data_source_block           b_f7
_cod_original_cell_volume        1264.02(4)
_cod_database_code               7019934