Versatile synthesis of chiral 6-oxoverdazyl radical ligands - new building blocks for multifunctional molecule-based magnets.
Solea, Atena B.; Wohlhauser, Tobie; Abbasi, Parisa; Mongbanziama, Yvan; Crochet, Aurelien; Fromm, Katharina M.; Novitchi, Ghenadie; Train, Cyrille; Pilkington, Melanie; Mamula, Olimpia; Dalton transactions (Cambridge, England : 2003) 47 (2018) 4785–4789; doi:10.1039/c8dt00840j

data_7045780
_publ_section_title
;
 Versatile synthesis of chiral 6-oxoverdazyl radical ligands - new
 building blocks for multifunctional molecule-based magnets.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4785
_journal_page_last               4789
_journal_paper_doi               10.1039/c8dt00840j
_journal_volume                  47
_journal_year                    2018
_chemical_absolute_configuration syn
_chemical_formula_moiety         '2(C20 H28 Cl2 Cu N5 O)'
_chemical_formula_sum            'C20 H28 Cl2 Cu N5 O'
_chemical_formula_weight         488.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-12-14 deposited with the CCDC.
2018-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.955(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0978(9)
_cell_length_b                   11.0063(7)
_cell_length_c                   16.8554(14)
_cell_measurement_reflns_used    4951
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.03
_cell_measurement_theta_min      1.26
_cell_volume                     2336.2(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3274
_diffrn_reflns_av_unetI/netI     0.2514
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30974
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.196
_diffrn_reflns_theta_max         25.196
_diffrn_reflns_theta_min         1.256
_diffrn_source
'sealed X-ray tube, 12x0.4 mm long-fine focus'
_diffrn_source_type              'Stoe IPDS2'
_exptl_absorpt_coefficient_mu    1.184
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.7442
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in
F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_recrystallization_method Ethanol
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.02(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         8335
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.2226
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0716P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.2174
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                2991
_reflns_number_total             8335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00840j2.cif
_cod_data_source_block           ATE80
_cod_depositor_comments
'Adding full bibliography for 7045778--7045781.cif.'
_cod_database_code               7045780
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              62164