Redox induced oxidative C-C coupling of non-innocent bis(heterocyclo)methanides
Lahiri, Goutam Kumar; Panda, Sanjib; Baliyan, Rupal; Dhara, Suman; Huang, Kuo-Wei; Dalton Transactions  (2021) –; doi:10.1039/D1DT03310G

data_7708775
_publ_section_title
;
 Redox induced oxidative C-C coupling of non-innocent
 bis(heterocyclo)methanides
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03310G
_journal_year                    2021
_chemical_formula_moiety         'C38 H34 N8 O8 Zn2, 2(H2 O)'
_chemical_formula_sum            'C38 H38 N8 O10 Zn2'
_chemical_formula_weight         897.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-10-11
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-10-14 deposited with the CCDC.	2021-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                63.830(5)
_cell_angle_beta                 87.600(4)
_cell_angle_gamma                75.968(4)
_cell_formula_units_Z            1
_cell_length_a                   8.9786(4)
_cell_length_b                   10.6986(4)
_cell_length_c                   11.1021(6)
_cell_measurement_reflns_used    5051
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.0500
_cell_measurement_theta_min      2.1970
_cell_volume                     925.97(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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   -110.00  25.00   0.50    8.00    --  -20.00   0.00  36.00  270
  2  \w   -110.00  10.00   0.50    8.00    --  -20.00 -72.00  36.00  240
  3  \w    -64.50  19.00   0.50    8.00    --  -20.00 -72.00-180.00  167
  4  \w    -34.00 -18.50   0.50    8.00    --  -20.00 -72.00-108.00   31
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6301
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.943
_exptl_absorpt_coefficient_mu    1.367
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       block
_exptl_crystal_F_000             462
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         3217
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0515P)^2^+0.3773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2805
_reflns_number_total             3217
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03310g2.cif
_cod_data_source_block           1b
_cod_original_cell_volume        925.98(8)
_cod_database_code               7708775
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.791
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.0005 and sigma for
terminal atoms of 0.0005
3.a Free rotating group:
 O5(H5A,H5B)
3.b Ternary CH refined with riding coordinates:
 C2(H2)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C6(H6), C14(H14), C4(H4), C15(H15), C13(H13), C7(H7),
 C8(H8), C9(H9)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              88293
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;