A detailed NMR study of the solution stereodynamics in tricarbonylrhenium(I) halide complexes of the non-racemic chiral ligand 2,6-bis[(4R,5R)-dimethyl-1,3-dioxan-2-yl]pyridine (L1) and the molecular structure of fac-[ReBr(CO)3(L1)] †
Heard, Peter J.; King, Paul M.; Bain, Alex. D.; Hazendonk, Paul; Tocher, Derek A.; Journal of the Chemical Society, Dalton Transactions  (1999) 4495–; doi:10.1039/a904026i

data_7027561
_publ_section_title
;
 A detailed NMR study of the solution stereodynamics in
 tricarbonylrhenium(I) halide complexes of the non-racemic chiral ligand
 2,6-bis[(4R,5R)-dimethyl-1,3-dioxan-2-yl]pyridine (L1) and the molecular
 structure of fac-[ReBr(CO)3(L1)]&#x200A;&#x2020;
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_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4495
_journal_paper_doi               10.1039/a904026i
_journal_year                    1999
_chemical_formula_sum            'C18 H21 Br N O7 Re'
_chemical_formula_weight         629.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 106.06(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.231(2)
_cell_length_b                   11.296(2)
_cell_length_c                   10.975(2)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      7
_cell_volume                     1099.7(4)
_computing_cell_refinement       'Nicolet R3'
_computing_data_collection       'Nicolet R3'
_computing_data_reduction        XDISK
_computing_molecular_graphics    XP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nicolet P3'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4083
_diffrn_reflns_theta_max         25.29
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        negligable
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.378
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.19
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.72
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.999
_refine_diff_density_min         -1.537
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.030
_refine_ls_goodness_of_fit_obs   0.996
_refine_ls_hydrogen_treatment    'fixed positions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3826
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_restrained_S_obs      0.996
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_obs          0.0435
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+8.2712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1225
_refine_ls_wR_factor_obs         0.1082
_reflns_number_observed          3501
_reflns_number_total             3832
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            904026Isup1.cif
_cod_data_source_block           str635
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Psi scan'
changed to 'psi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+8.2712P] 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^)+(0.0666P)^2^+8.2712P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7027561