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_4103316
_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           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 101.80(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.990(2)
_cell_length_b                   12.734(2)
_cell_length_c                   18.542(2)
_cell_measurement_reflns_used    8191
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      2.5
_cell_volume                     2540.1(7)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
A full sphere of reciprocal space was scanned by 0.3\% \w steps, collecting
2400 frames each at 10 s exposure keeping the detector at 6.6 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  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19242
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    9.859
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.258
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Sheldrick, G. M. (1996). SADABS. Universit\"at G\"ottingen, Germany.
Reflections employed for parameter determination: 13714
Maximum odd and even orders for spherical harmonics: 7 and 8
Effective data to parameter ratio: 4.8
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1560
_exptl_crystal_preparation
;
Crystals were obtained by slow diffusion of n-hexane in a dichloromethane
solution at 248 K.
;
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.195
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         3042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0194
_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^)+(0.015P)^2^+4.1P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0348
_refine_ls_wR_factor_ref         0.0359
_reflns_number_gt                2760
_reflns_number_total             3042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja106772v_si_002.cif
_cod_data_source_block           1yellow
_cod_database_code               4103316