Tricarbonylrhenium(I) halide complexes of 2-[(4R,6R)-4,6-dimethyl-1,3-dioxan-2-yl]pyridine (L1) and 2,6-bis[(4R,6R)-4,6-dimethyl-1,3-dioxan-2-yl]pyridine (L2): structure and solution stereodynamics
Heard, Peter J.; King, Paul M.; Tocher, Derek A.; Journal of the Chemical Society, Dalton Transactions  (2000) 1769–; doi:10.1039/b001206h

data_7009456
_publ_section_title
;
 Tricarbonylrhenium(I) halide complexes of
 2-[(4R,6R)-4,6-dimethyl-1,3-dioxan-2-yl]pyridine (L1) and
 2,6-bis[(4R,6R)-4,6-dimethyl-1,3-dioxan-2-yl]pyridine (L2): structure
 and solution stereodynamics
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_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1769
_journal_paper_doi               10.1039/b001206h
_journal_year                    2000
_chemical_formula_sum            'C20 H25 Br N O7 Re'
_chemical_formula_weight         657.52
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           154
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.438(2)
_cell_length_b                   14.438(2)
_cell_length_c                   19.673(4)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      7.5
_cell_volume                     3551.5(10)
_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 R3mV'
_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  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4700
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.858
_exptl_absorpt_correction_T_max  0.21
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   'psi scans'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_description       block
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.47
_refine_diff_density_max         0.814
_refine_diff_density_min         -1.377
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.007
_refine_ls_goodness_of_fit_obs   1.028
_refine_ls_hydrogen_treatment    'fixed contribution'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         2363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_restrained_S_obs      1.028
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_obs          0.0348
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0856
_refine_ls_wR_factor_obs         0.0814
_reflns_number_observed          2141
_reflns_number_total             2366
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b001206h.txt
_cod_data_source_block           str671
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.0000P] 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^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct Methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      P3(2)2(1)
_cod_database_code               7009456