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_7031981
_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
'C52 H58 Cu F12 N4 O8 P2, 2(C31 H30 Cu F12 N2 O6 P), 2(C7 H16)'
_chemical_formula_sum            'C128 H150 Cu3 F36 N8 O20 P4'
_chemical_formula_weight         3119.09
_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
_audit_creation_date             2014-02-26T16:29:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 99.114(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0520(3)
_cell_length_b                   30.2136(7)
_cell_length_c                   20.5874(6)
_cell_measurement_reflns_used    20077
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      29.4924
_cell_measurement_theta_min      1.8356
_cell_volume                     7401.9(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      120(1)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_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  0.0638
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            83125
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.889
_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            green
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3210
_exptl_crystal_size_max          0.0802
_exptl_crystal_size_mid          0.0583
_exptl_crystal_size_min          0.0304
_refine_diff_density_max         1.364
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         13082
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+17.8403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1563
_reflns_number_gt                9957
_reflns_number_total             13082
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01444h2.cif
_cod_data_source_block           cuhfacrades
_cod_depositor_comments
'Adding full bibliography for 7031981--7031984.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7031981