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_7019932
_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 Ni, 0.5(C6 H12)'
_chemical_formula_sum            'C33 H48 Ni'
_chemical_formula_weight         503.42
_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_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                92.056(2)
_cell_angle_beta                 99.017(2)
_cell_angle_gamma                97.933(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0461(3)
_cell_length_b                   11.0398(4)
_cell_length_c                   12.8487(3)
_cell_measurement_reflns_used    15445
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      31.0309
_cell_measurement_theta_min      3.5246
_cell_volume                     1391.52(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.7 (release 14-02-2011 CrysAlis171 .NET)
(compiled Feb 15 2011,09:34:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.7 (release 14-02-2011 CrysAlis171 .NET)
(compiled Feb 15 2011,09:34:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.7 (release 14-02-2011 CrysAlis171 .NET)
(compiled Feb 15 2011,09:34:54)
;
_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      100.0
_diffrn_detector_area_resol_mean 10.3347
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
1 omega -93.00 -16.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- -15.0548 155.0000 -60.0000 77

2 omega -76.00 -1.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- -15.0548 131.0000 138.0000 75

3 omega -75.00 -47.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- -15.0548 129.0000 -108.0000 28

4 omega -93.00 17.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- -15.0548 -77.0000 -180.0000 110

5 omega -81.00 11.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- -15.0548 -38.0000 -90.0000 92

6 omega -33.00 61.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- -15.0548 38.0000 -60.0000 94

7 omega -93.00 19.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- -15.0548 -77.0000 30.0000 112

8 omega -57.00 48.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- 15.3673 -77.0000 90.0000 105

9 omega -91.00 11.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- -15.0548 -38.0000 30.0000 102

10 omega -91.00 11.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- -15.0548 -38.0000 -60.0000 102

11 omega -104.00 -32.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- -15.0548 179.0000 -150.0000 72

12 omega -91.00 11.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- -15.0548 -38.0000 -180.0000 102

13 omega 22.00 76.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- 15.3673 -131.0000 -174.0000 54

14 omega -61.00 42.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- 15.3673 -38.0000 90.0000 103

15 omega -75.00 0.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- -15.0548 129.0000 -108.0000 75

16 omega -85.00 -10.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- -15.0548 146.0000 161.0000 75

17 omega -72.00 4.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- -15.0548 124.0000 38.0000 76

18 omega 56.00 105.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- 15.3673 179.0000 60.0000 49

19 omega -11.00 91.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- 15.3673 38.0000 60.0000 102

20 omega -18.00 94.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- 15.3673 77.0000 120.0000 112

21 omega -74.00 99.00 1.0000 29.9900
omega____ theta____ kappa____ phi______ frames
- 15.3673 0.0000 -180.0000 173
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0603938000
_diffrn_orient_matrix_UB_12      0.0246056000
_diffrn_orient_matrix_UB_13      -0.0184447000
_diffrn_orient_matrix_UB_21      -0.0375907000
_diffrn_orient_matrix_UB_22      -0.0598171000
_diffrn_orient_matrix_UB_23      -0.0056674000
_diffrn_orient_matrix_UB_31      -0.0126735000
_diffrn_orient_matrix_UB_32      0.0062548000
_diffrn_orient_matrix_UB_33      0.0525619000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            55175
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.53
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.7 (release 14-02-2011 CrysAlis171 .NET)
(compiled Feb 15 2011,09:34:54)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+1.4049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                4278
_reflns_number_total             4879
_reflns_threshold_expression     I>2u(I)
_cod_data_source_file            c2dt31291c.txt
_cod_data_source_block           b2_c
_cod_database_code               7019932