Microwave and solvothermal methods for the synthesis of nickel and ruthenium complexes with 9-anthracene carboxylate ligand
Cortijo, Miguel; Delgado-Martínez, Patricia; González-Prieto, Rodrigo; Herrero, Santiago; Jiménez-Aparicio, Reyes; Perles, Josefina; Priego, José L.; Torres, M. R.; Inorganica Chimica Acta 424 (2015) 176–185; doi:10.1016/j.ica.2014.07.063

data_1518848
_publ_section_title
;
 Microwave and solvothermal methods for the synthesis of nickel and
 ruthenium complexes with 9-anthracene carboxylate ligand
;
_journal_coden_ASTM              ICHAA3
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              176
_journal_page_last               185
_journal_paper_doi               10.1016/j.ica.2014.07.063
_journal_volume                  424
_journal_year                    2015
_chemical_formula_sum            'C68 H58 O12 Ru2'
_chemical_formula_weight         1269.28
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 95.357(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1375(2)
_cell_length_b                   18.2232(5)
_cell_length_c                   17.7988(5)
_cell_measurement_reflns_used    7469
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5219
_cell_measurement_theta_min      3.3538
_cell_volume                     2950.81(13)
_computing_cell_refinement
; 
'Wed May 21 10:29:08 2014' 
;
_computing_data_collection
; 
'Wed May 21 10:29:08 2014' 
;
_computing_data_reduction
; 
'Wed May 21 10:29:08 2014' 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3317
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22862
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
'Wed May 21 10:29:08 2014' 
;
_exptl_crystal_colour            'translucent dark brown'
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.4800
_exptl_crystal_size_mid          0.2400
_exptl_crystal_size_min          0.2000
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5793
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.9881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                4538
_reflns_number_total             5793
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2015-424176-185-1.cif
_cod_data_source_block           2pdm480
_cod_original_cell_volume        2950.82(14)
_cod_database_code               1518848