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_7045781
_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         'C13 H15 N O'
_chemical_formula_sum            'C13 H15 N O'
_chemical_formula_weight         201.26
_chemical_name_systematic
(6R,8R)-7,7-dimethyl-5,6,7,8-tetrahydro-6,8-methanoisoquinoline-3-carbaldehyde
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      96
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.5168(4)
_cell_length_b                   7.5168(4)
_cell_length_c                   39.316(2)
_cell_measurement_reflns_used    8511
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.78
_cell_measurement_theta_min      2.07
_cell_volume                     2221.4(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.1169
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            28194
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.156
_diffrn_reflns_theta_max         25.156
_diffrn_reflns_theta_min         2.072
_diffrn_source                   'sealed X-ray tube, 12x0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.9911
_exptl_absorpt_correction_T_min  0.9543
_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            yellow
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       cube
_exptl_crystal_F_000             864
_exptl_crystal_recrystallization_method ethylacetate
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.205
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
The Flack parameter was meaningless, -3(5), and has been erased.
;
_refine_ls_extinction_coef       0.020(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.384
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1977
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.384
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0507
_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=exp[3.0000(sin\q/\l)^2^)]/[\s^2^(Fo^2^)+(0.0892P)^2^+0.0400] where P=(0.1000Fo^2^+0.9000Fc^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1564
_reflns_Friedel_coverage         0.563
_reflns_Friedel_fraction_full    1.001
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1336
_reflns_number_total             1977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00840j2.cif
_cod_data_source_block           45-ald
_cod_depositor_comments
'Adding full bibliography for 7045778--7045781.cif.'
_cod_original_cell_volume        2221.4(3)
_cod_database_code               7045781
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.990
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              31704