Preparation, Characterization, and Luminescence Properties of Gallium-Metal Face-to-Face Diporphyrins (M = H2, GaL, Ru(CO)(OH), Co)
Pierre D. Harvey; Nathalie Proulx; Geneviève Martin; Marc Drouin; Daniel J. Nurco; Kevin M. Smith; Frédéric Bolze; Claude P. Gros; Roger Guilard; Inorganic Chemistry 40 (2001) 4134–4142; doi:10.1021/ic001446j

data_4320046
_publ_section_title
;
 Preparation, Characterization, and Luminescence Properties of
 Gallium-Metal Face-to-Face Diporphyrins (M = H2, GaL, Ru(CO)(OH), Co)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4134
_journal_page_last               4142
_journal_paper_doi               10.1021/ic001446j
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety
;
    2(C81 H85 Ga N8 O3 Ru), 0.53(C4 H8 O), 1.21(C7 H8), 3.82(H2 O)
;
_chemical_formula_sum            'C172.59 H191.56 Ga2 N16 O7.35 Ru2'
_chemical_formula_weight         2949.33
_chemical_name_common            'DPA [GaOMe][MeHO-Ru-CO]'
_chemical_name_systematic
;
    ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.38(3)
_cell_angle_beta                 96.02(3)
_cell_angle_gamma                94.02(3)
_cell_formula_units_Z            4
_cell_length_a                   18.946(4)
_cell_length_b                   21.535(4)
_cell_length_c                   21.572(4)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      14.12
_cell_measurement_theta_min      3.15
_cell_volume                     8305(3)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        XDISK
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  'Bruker SHELXTL V. 5.03'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.717
_diffrn_measured_fraction_theta_max 0.717
_diffrn_measurement_device_type  'Bruker R3/mV'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1623
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21055
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2938
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.00064(13)
_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   1.021
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1753
_refine_ls_number_reflns         20991
_refine_ls_number_restraints     509
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.2059
_refine_ls_R_factor_gt           0.0998
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1527P)^2^+6.7709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2428
_refine_ls_wR_factor_ref         0.3169
_reflns_number_gt                9811
_reflns_number_total             21055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001446j_4.cif
_cod_data_source_block           rgk62j
_cod_original_formula_sum
;
    C172.59 H191.56 Ga2 N16 O7.35 Ru2
;
_cod_database_code               4320046