Luminescent Rhenium(I)-Dipyrrinato Complexes
Tracey M. McLean; Janice L. Moody; Mark R. Waterland; Shane G. Telfer; Inorganic Chemistry 51 (2012) 446–455; doi:10.1021/ic201877t

data_4327831
_publ_section_title
;
 Luminescent Rhenium(I)-Dipyrrinato Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              446
_journal_page_last               455
_journal_paper_doi               10.1021/ic201877t
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C56 H47 N2 O2 P2 Re'
_chemical_formula_weight         1028.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 102.342(7)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   16.4699(3)
_cell_length_b                   13.1498(2)
_cell_length_c                   23.4400(16)
_cell_measurement_reflns_used    27731
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      72.11
_cell_measurement_theta_min      6.71
_cell_volume                     4959.2(4)
_computing_cell_refinement       'FS Process (Rigaku, 1998)'
_computing_data_collection       'Crystal Clear (Rigaku, 2005)'
_computing_data_reduction        'FS Process (Rigaku, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      'X images in steps of Y\%'
_diffrn_measurement_device_details 'Curved image plate'
_diffrn_measurement_device_type  'Rigaku Spider'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  'confocal optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_sigmaI/netI    0.0867
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28154
_diffrn_reflns_theta_full        54.24
_diffrn_reflns_theta_max         54.24
_diffrn_reflns_theta_min         6.71
_exptl_absorpt_coefficient_mu    5.725
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            Plate
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       Orange
_exptl_crystal_F_000             2072.00
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
Attempts to model the solvent with chemically sensible species failed. 
The badly disordered solvent was removed by means of the SQUEEZE option 
in the PLATON suite. Subsequent refinement lead to a lower R and 
especially wR2. 
;
_refine_diff_density_max         1.755
_refine_diff_density_min         -1.102
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         5904
_refine_ls_number_restraints     487
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+6.3730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                4889
_reflns_number_total             5904
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201877t_si_002_11.cif
_cod_data_source_block           3D
_cod_original_cell_volume        4959.3
_cod_database_code               4327831