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_1518849
_publ_section_title
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 Microwave and solvothermal methods for the synthesis of nickel and
 ruthenium complexes with 9-anthracene carboxylate ligand
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_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            'C44 H44 N2 Ni O8'
_chemical_formula_weight         787.52
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 93.455(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2501(8)
_cell_length_b                   15.5220(14)
_cell_length_c                   31.598(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4039.0(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0735
_diffrn_reflns_av_sigmaI/netI    0.0791
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            35411
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.535
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1656
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         8819
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1472
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+2.4792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1677
_reflns_number_gt                4082
_reflns_number_total             8819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2015-424176-185-2.cif
_cod_data_source_block           sad
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1518849