A Crystalline Monomeric Allenyl/Propargyl Radical.
Hansmann, Max M.; Melaimi, Mohand; Bertrand, Guy; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b09622

data_4126645
_publ_section_title
;
 A Crystalline Monomeric Allenyl/Propargyl Radical.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b09622
_journal_year                    2017
_chemical_formula_moiety         'C40 H50 Co N'
_chemical_formula_sum            'C40 H50 Co N'
_chemical_formula_weight         603.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-08-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_cell_angle_alpha                86.599(2)
_cell_angle_beta                 75.345(2)
_cell_angle_gamma                75.325(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3348(5)
_cell_length_b                   10.9124(5)
_cell_length_c                   17.2615(8)
_cell_measurement_reflns_used    9114
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.981
_cell_measurement_theta_min      2.646
_cell_volume                     1645.62(14)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX3 v2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Platinum135 CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Platinum135'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49417
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         70.067
_diffrn_reflns_theta_min         2.646
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker FR-591'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.278
_exptl_absorpt_correction_T_max  0.5231
_exptl_absorpt_correction_T_min  0.3937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0742 before and 0.0562 after correction. The Ratio of minimum to maximum transmission is 0.7526. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       needle
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         6159
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.5970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6044
_reflns_number_total             6159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            6a.cif
_cod_data_source_block           gb_mhvdi
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               4126645
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.521
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C36A, C40A, C39A, C38A, C37A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Others
 Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39A)=Sof(C40A)=
 Sof(H40A)=Sof(C36A)=Sof(H36A)=1-FVAR(1)
 Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37)=
 Sof(C38)=Sof(H38)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C36A(H36A)
4.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C3(H3A,H3B), C21(H21A,H21B)
4.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C27(H27), C30(H30), C26(H26), C8(H8), C28(H28), C39(H39),
 C40(H40), C29(H29), C36(H36), C37(H37), C38(H38), C37A(H37A), C38A(H38A),
 C39A(H39A), C40A(H40A)
4.d Fitted pentagon refined as free rotating group:
 C37A(C38A,C39A,C40A,C36A)
4.e Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C12(H12A,H12B,H12C), C22(H22A,
 H22B,H22C)
;
_shelx_res_checksum              51664
_shelx_hkl_checksum              76530
_olex2_submission_special_instructions 'No special instructions were received'