Synthesis and Reactions of fac-[Re(dmbpy)(CO)3X] (dmbpy \δb 4,4'-Dimethyl-2,2'-bipyridine; X =COOH, CHO) and Their Derivatives
Dorothy H. Gibson; Xiaolong Yin; Haiyang He; Mark S. Mashuta; Organometallics 22 (2003) 337–346; doi:10.1021/om020677q

data_4060674
_publ_section_title
;
 Synthesis and Reactions of fac-[Re(dmbpy)(CO)3X] (dmbpy \\db
 4,4'-Dimethyl-2,2'-bipyridine; X \\db COOH, CHO) and Their Derivatives
;
_journal_name_full               Organometallics
_journal_page_first              337
_journal_page_last               346
_journal_paper_doi               10.1021/om020677q
_journal_volume                  22
_journal_year                    2003
_chemical_formula_moiety
'C48 H48 N6 O12 Re3, RE O4, 0.75(C Cl2), 0.25(C2 O)'
_chemical_formula_sum            'C49.25 H48 Cl1.5 N6 O16.25 Re4'
_chemical_formula_weight         1776.82
_chemical_name_common            '[fac-Re(dmbpy)(CO)~3~]3(OCO~2~)ReO~4~'
_chemical_name_systematic
; 
 [fac-Re(dmbpy)(CO)~3~]3(OCO~2~)ReO~4~
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
  
  April_11_2002 text and data added by Mark S. Mashuta
  August_8_2002 text and data added by Mark S. Mashuta
;
_cell_angle_alpha                90.00
_cell_angle_beta                 123.571(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   40.977(5)
_cell_length_b                   13.1061(18)
_cell_length_c                   23.985(3)
_cell_measurement_reflns_used    12472
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      1.66
_cell_volume                     10732(2)
_computing_cell_refinement       'SAINT 6.22 (Bruker, 1994)'
_computing_data_collection       'SMART 5.625 (Bruker, 1994)'
_computing_data_reduction        'SAINT 6.22 (Bruker, 1994)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'SMART APEX CCD'
_diffrn_measurement_method       '\w scans'
_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  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            45501
_diffrn_reflns_theta_full        28.22
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    9.143
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M.; SADABS (1996).

;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.199
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             6660
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.850
_refine_diff_density_min         -4.091
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         12472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.052
_refine_ls_R_factor_gt           0.039
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+14.3487P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.103
_refine_ls_wR_factor_ref         0.111
_reflns_number_gt                10265
_reflns_number_total             12472
_reflns_threshold_expression     >2sigma(I)
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C49.25 H48 Cl1.50 N6 O16.25 Re4'
_cod_database_code               4060674