Norharmane rhenium(i) polypyridyl complexes: synthesis, structural and spectroscopic characterization.
Maisuls, Iván; Wolcan, Ezequiel; Piro, Oscar E.; Etcheverría, Gustavo A; Petroselli, Gabriela; Erra-Ballsels, Rosa; Cabrerizo, Franco M.; Ruiz, Gustavo T.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 17064–17074; doi:10.1039/c5dt02790j

data_7036409
_publ_section_title
;
 Norharmane rhenium(i) polypyridyl complexes: synthesis, structural and
 spectroscopic characterization.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17064
_journal_page_last               17074
_journal_paper_doi               10.1039/c5dt02790j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C25 H16 F3 N4 O6 Re S'
_chemical_formula_weight         743.68
_chemical_name_systematic
"fac-tricarbonyl(2,2' bipyridine)(9H-pyrido[3,4-b]indole)rhenium(I) trifluoromethanesulfonate"
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_Hall           'P 31'
_space_group_name_H-M_alt        'P 31'
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-08-14 deposited with the CCDC.
2015-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   15.1660(9)
_cell_length_b                   15.1660(9)
_cell_length_c                   9.9800(7)
_cell_measurement_reflns_used    15861
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      2.546
_cell_volume                     1987.9(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10339
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_min         2.686
_exptl_absorpt_coefficient_mu    4.6900
_exptl_absorpt_correction_T_max  0.7808
_exptl_absorpt_correction_T_min  0.5149
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
a grid of  8 x 8 x 8 = 512 sampling points was used
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1080
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichlomethane, iso-octane'
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.059
_refine_diff_density_max         1.444
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Flack x determined using 1693 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(15)
_refine_ls_extinction_coef       0.029(2)
_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_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         5145
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0917P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.972
_reflns_friedel_fraction_full    0.972
_reflns_friedel_fraction_max     0.970
_reflns_number_gt                4106
_reflns_number_total             5145
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02790j2.cif
_cod_data_source_block           '[Re(CO)3(bipy)(nHo)(CO)3]CF3SO3'
_cod_depositor_comments
'Adding full bibliography for 7036408--7036409.cif.'
_cod_original_cell_volume        1987.9(3)
_cod_database_code               7036409
_shelx_estimated_absorpt_t_min   0.435
_shelx_estimated_absorpt_t_max   0.768
_exptl_absorpt_correction_t_ave  0.7068
_shelxl_version_number           2014-3
_shelx_res_checksum              54653