Synthesis, crystal structures and magnetic behaviour of four coordination compounds constructed with a phosphinic amide-TEMPO radical and [M(hfac)2] (M = Cu(II), Co(II) and Mn(II)).
Reis, Samira G.; Del Águila-Sánchez, Miguel A; Guedes, Guilherme P.; Ferreira, Glaucio B.; Novak, Miguel A.; Speziali, Nivaldo L.; López-Ortiz, Fernando; Vaz, Maria G. F.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 14889–14901; doi:10.1039/c4dt01444h

data_7031982
_publ_section_title
;
 Synthesis, crystal structures and magnetic behaviour of four coordination
 compounds constructed with a phosphinic amide-TEMPO radical and
 [M(hfac)2] (M = Cu(II), Co(II) and Mn(II)).
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14889
_journal_page_last               14901
_journal_paper_doi               10.1039/c4dt01444h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C72 H62 Co3 F36 N4 O16 P2, 2(C7 H16)'
_chemical_formula_sum            'C86 H94 Co3 F36 N4 O16 P2'
_chemical_formula_weight         2362.39
_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_date             2014-02-26T17:14:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                79.807(5)
_cell_angle_beta                 86.092(5)
_cell_angle_gamma                73.575(6)
_cell_formula_units_Z            1
_cell_length_a                   13.0336(9)
_cell_length_b                   13.2483(9)
_cell_length_c                   16.6020(11)
_cell_measurement_reflns_used    2579
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5033
_cell_measurement_theta_min      1.9543
_cell_volume                     2705.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
Ortep-3 for Windows: L. J. Farrugia, J. Appl. Cryst (1997), 30, 565
;
_computing_publication_material
'WinGX publication routines (Farrugia, 1999) and Publcif'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_unetI/netI     0.1202
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16437
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  0.9980
_exptl_absorpt_correction_T_min  0.9680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.45
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1201
_exptl_crystal_size_max          0.1060
_exptl_crystal_size_mid          0.0803
_exptl_crystal_size_min          0.0514
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         8949
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1543
_refine_ls_R_factor_gt           0.0725
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0977P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.2207
_reflns_number_gt                4570
_reflns_number_total             9561
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01444h2.cif
_cod_data_source_block           exp_5447
_cod_depositor_comments
'Adding full bibliography for 7031981--7031984.cif.'
_cod_database_code               7031982