Stereoselective Synthesis of Chiral Pinene[5,6]bipyridine Ligands and Their Coordination Chemistry
Didier Lötscher; Stefan Rupprecht; Philippe Collomb; Peter Belser; Heiko Viebrock; Alex von Zelewsky; Peter Burger; Inorganic Chemistry 40 (2001) 5675–5681; doi:10.1021/ic010411w

data_4320391
_publ_section_title
;
 Stereoselective Synthesis of Chiral Pinene[5,6]bipyridine Ligands and
 Their Coordination Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5675
_journal_page_last               5681
_journal_paper_doi               10.1021/ic010411w
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C27 H34 N2'
_chemical_formula_weight         386.56
_chemical_name_common            (-)-Isopropyl-di-pinene-[5,6]-bipyridine
_space_group_IT_number           19
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.722(4)
_cell_length_b                   13.050(6)
_cell_length_c                   26.141(13)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      19
_cell_volume                     2293(2)
_computing_cell_refinement       'Siemens P3-program'
_computing_data_collection       'Siemens P3-program'
_computing_data_reduction        'Siemens XDISK-Program'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P3'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0699
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            5566
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         2.21
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.168
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -3.13(615)
_refine_ls_extinction_coef       0.0000(34)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.077
_refine_ls_goodness_of_fit_obs   1.162
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_restrained_S_obs      1.162
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_obs          0.0833
_refine_ls_shift/esd_max         -1.927
_refine_ls_shift/esd_mean        0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+0.8924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2009
_refine_ls_wR_factor_obs         0.1773
_reflns_number_observed          3414
_reflns_number_total             4704
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010411w_1.cif
_cod_data_source_block           r01
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+0.8924P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+0.8924P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2293.1(21)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               4320391