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_1518850
_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            'C80 H56 N4 Ni2 O9.5'
_chemical_formula_weight         1342.67
_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
_cell_angle_alpha                112.072(4)
_cell_angle_beta                 98.823(5)
_cell_angle_gamma                97.444(5)
_cell_formula_units_Z            4
_cell_length_a                   16.910(3)
_cell_length_b                   19.838(5)
_cell_length_c                   22.694(5)
_cell_measurement_temperature    293(2)
_cell_volume                     6824(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.2252
_diffrn_reflns_av_sigmaI/netI    0.4760
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            53996
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    0.614
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2784
_refine_diff_density_max         1.202
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.202
_refine_ls_extinction_coef       0.0386(18)
_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   0.902
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1730
_refine_ls_number_reflns         24280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.3344
_refine_ls_R_factor_gt           0.1118
_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^)+(0.1310P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2388
_refine_ls_wR_factor_ref         0.3626
_reflns_number_gt                6223
_reflns_number_total             24280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2015-424176-185-3.cif
_cod_data_source_block           sad
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

2019-07-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        6825(3)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C160 H112 N8 Ni4 O19'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     2685.34
_cod_database_code               1518850