Expanding the Boxmi Ligand Family: Synthesis and Application of New NON and NSN Ligands.
Blasius, Clemens; Ren, Bing-Tao; Bürgy, David; Liu, Yan-Kai; Li, Bin; Michalsky, Ina; Wadepohl, Hubert; Deng, Qing-Hai; Gade, Lutz H.; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.0c00751

data_4038296
_publ_section_title
;
 Expanding the Boxmi Ligand Family: Synthesis and Application of New NON
 and NSN Ligands.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c00751
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H26 Cl2 Co N2 O3'
_chemical_formula_sum            'C30 H26 Cl2 Co N2 O3'
_chemical_formula_weight         592.36
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_cb16
_audit_creation_date             2019-01-22
_audit_creation_method
;
encif (version 1.112)

encifer (version_id = 270009.64)

Olex2 1.3
(compiled 2019.11.22 svn.r41b7951 for OlexSys, GUI svn.r6003)
;
_audit_update_record
'19.02.2020 11:16:14 CET UTC+01:00  encif 1.112'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5248(2)
_cell_length_b                   9.9876(3)
_cell_length_c                   34.3832(8)
_cell_measurement_reflns_used    9715
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      27.3630
_cell_measurement_theta_min      2.9390
_cell_volume                     2584.06(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_publication_material
'encif (Wadepohl, 2009-19); encifer (Allen et al., 2004)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -20.00  72.00   0.50   17.50    --   28.16 -99.00-180.00  184
  2  \w     -3.00  99.00   0.50   17.50    --   28.16  77.00 -60.00  204
  3  \w      7.00  97.00   0.50   17.50    --   28.16  57.00-180.00  180
  4  \w    -41.00  50.00   0.50   17.50    --   28.16 -57.00  30.00  182
  5  \w    -20.00  72.00   0.50   17.50    --   28.16 -99.00 -30.00  184
  6  \w     -3.00  99.00   0.50   17.50    --   28.16  77.00  60.00  204
  7  \w    -99.00   4.00   0.50   17.50    --  -28.08 -77.00 120.00  206
  8  \w      7.00  97.00   0.50   17.50    --   28.16  57.00 -90.00  180
  9  \w    -20.00  72.00   0.50   17.50    --   28.16 -99.00 120.00  184
 10  \w      7.00  97.00   0.50   17.50    --   28.16  57.00  30.00  180
 11  \w    -44.00  56.00   0.50   17.50    --   28.16 -38.00-180.00  200
 12  \w   -101.00 -76.00   0.50   17.50    --  -28.08 -38.00 150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Agilent SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0360128000
_diffrn_orient_matrix_UB_12      0.0648580000
_diffrn_orient_matrix_UB_13      0.0029130000
_diffrn_orient_matrix_UB_21      -0.0506593000
_diffrn_orient_matrix_UB_22      -0.0068531000
_diffrn_orient_matrix_UB_23      -0.0172755000
_diffrn_orient_matrix_UB_31      -0.0708320000
_diffrn_orient_matrix_UB_32      -0.0281134000
_diffrn_orient_matrix_UB_33      0.0109010000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.1117
_diffrn_reflns_av_unetI/netI     0.1334
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            51027
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.322
_diffrn_reflns_theta_min         2.358
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 1517 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.841
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         10294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.841
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0227P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.750
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                6526
_reflns_number_total             10294
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.7697\%
 around [0.01 1.00 -0.01] (reciprocal) or [0.02 1.00 -0.00] (direct)
;
_cod_data_source_file            jo0c00751_si_002.cif
_cod_data_source_block           ga_cb16_5
_cod_original_cell_volume        2584.08(13)
_cod_database_code               4038296
_audit_block_refno               3250
_audit_block_usercomment         'CBIM02, irregular, green'
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.915
_shelxl_version_number           2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.641(2)
 0.359(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C1(H1), C16(H16)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C15(H15A,H15B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8), C9(H9), C13(H13), C18(H18), C19(H19), C20(H20), C21(H21),
 C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
3.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_shelx_res_checksum              3975
_cell_oxdiff_length_a            7.5268(4)
_cell_oxdiff_length_b            9.9873(5)
_cell_oxdiff_length_c            34.3754(6)
_cell_oxdiff_angle_alpha         90.034(3)
_cell_oxdiff_angle_beta          89.945(3)
_cell_oxdiff_angle_gamma         90.024(4)
_cell_oxdiff_volume              2584.1(2)
_cell_oxdiff_measurement_reflns_used 9715