Highly Emitting Concomitant Polymorphic Crystals of a Dinuclear Rhenium Complex
Elsa Quartapelle Procopio; Matteo Mauro; Monica Panigati; Daniela Donghi; Pierluigi Mercandelli; Angelo Sironi; Giuseppe D'Alfonso; Luisa De Cola; Journal of the American Chemical Society 132 (2010) 14397–14399; doi:10.1021/ja106772v

data_4103317
_publ_section_title
;
 Highly Emitting Concomitant Polymorphic Crystals of a Dinuclear Rhenium
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14397
_journal_page_last               14399
_journal_paper_doi               10.1021/ja106772v
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C16 H20 Cl2 N2 O6 Re2 Si2'
_chemical_formula_sum            'C16 H20 Cl2 N2 O6 Re2 Si2'
_chemical_formula_weight         835.82
_chemical_name_systematic
;
hexacarbonyldi-\m-chloro(\m-4,5-bis(trimethylsilyl)pyridazine-\kN1:\kN2)
dirhenium
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.509(2)
_cell_length_b                   6.355(2)
_cell_length_c                   36.997(2)
_cell_measurement_reflns_used    8676
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.9
_cell_measurement_theta_min      2.2
_cell_volume                     5057.1(17)
_computing_structure_refinement
;
Sheldrick, G. M. (1997). SHELX97. Universit\"at G\"ottingen, Germany.
;
_computing_structure_solution
;
SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L.,
Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. &
Spagna, R. (1999). J. Appl. Crystallogr. 32, 115-119.
;
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
A full sphere of reciprocal space was scanned by 0.3\% \w steps, collecting
2400 frames each at 20 s exposure keeping the detector at 7.0 cm from the
sample. Intensity decay was monitored by recollecting the initial 50 frames
at the end of data collection and analysing the duplicate reflections.
;
_diffrn_measurement_device_type  'Brucker APEX II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            60064
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.10
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    9.904
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.167
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Sheldrick, G. M. (1996). SADABS. Universit\"at G\"ottingen, Germany.
Reflections employed for parameter determination: 43564
Maximum odd and even orders for spherical harmonics: 7 and 8
Effective data to parameter ratio: 10.4
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3120
_exptl_crystal_preparation
;
Crystals were obtained by slow diffusion of n-hexane in a dichloromethane
solution at 248 K.
;
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.293
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details
;
Flack, H. D. (1983). Acta Crystallogr., Sect. A 39, 876-881.
5803 Friedel pairs measured.
;
_refine_ls_abs_structure_Flack   0.354(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         10808
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.045P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                9908
_reflns_number_total             10808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja106772v_si_003.cif
_cod_data_source_block           1orange
_cod_database_code               4103317