Bicyclic (alkyl)(amino)carbene stabilized zinc(0) complex with singlet biradicaloid ground state.
Rajendran, N. M.; Gautam, Nimisha; Sarkar, Pallavi; Ahmed, Jasimuddin; Das, Arpan; Das, Shubhajit; Pati, Swapan K.; Mandal, Swadhin K.; Chemical communications (Cambridge, England) 57 (2021) 5282–5285; doi:10.1039/d1cc01298c

data_7128226
_publ_section_title
;
 Bicyclic (alkyl)(amino)carbene stabilized zinc(0) complex with singlet
 biradicaloid ground state.
;
_journal_issue                   43
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5282
_journal_page_last               5285
_journal_paper_doi               10.1039/d1cc01298c
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C44 H66 Cl4 N2 Zn2, 1.5[C7H8]'
_chemical_formula_sum            'C54.5 H78 Cl4 N2 Zn2'
_chemical_formula_weight         1033.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-03-23
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.03.16 svn.rd6aaa9fc for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-03-31 deposited with the CCDC.	2021-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.979(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6552(7)
_cell_length_b                   17.3124(13)
_cell_length_c                   15.8733(13)
_cell_measurement_reflns_used    3654
_cell_measurement_temperature    293.0
_cell_measurement_theta_max      25.0730
_cell_measurement_theta_min      2.0940
_cell_volume                     2613.2(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   35.00  121.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       26.7184  178.0000  -60.0000 86

  2 omega  -29.00  108.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       26.7184   38.0000    0.0000 137

  3 omega   35.00  121.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       26.7184  178.0000  150.0000 86

  4 omega  -11.00   14.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       26.7184   57.0000 -150.0000 25

  5 omega  -11.00  103.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       26.7184   57.0000  120.0000 114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14705
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.023
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         1.755
_exptl_absorpt_coefficient_mu    1.159
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       block
_exptl_crystal_F_000             1094
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4614
_refine_ls_number_restraints     274
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0679P)^2^+0.0802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3421
_reflns_number_total             4614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01298c2.cif
_cod_data_source_block           mr_1
_cod_depositor_comments
'Adding full bibliography for 7128226--7128227.cif.'
_cod_original_formula_sum        'C54.50 H78 Cl4 N2 Zn2'
_cod_database_code               7128226
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.801
_shelx_estimated_absorpt_t_min   0.654
_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) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=1-FVAR(1)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
 Sof(C2B)=Sof(C3B)=Sof(H3B)=Sof(H4BC)=Sof(H4BD)=Sof(H7BC)=Sof(H7BD)=Sof(C8B)=
 Sof(H8BA)=Sof(H8BB)=Sof(C10B)=Sof(H10A)=Sof(H10B)=Sof(H10C)=1-FVAR(2)
 Sof(H4AA)=Sof(H4AB)=Sof(H7AA)=Sof(H7AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C2A)=
 Sof(C8A)=Sof(H8A)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C3B(H3B), C17(H17), C20(H20), C8A(H8A)
4.b Secondary CH2 refined with riding coordinates:
 C4(H4BC,H4BD), C4(H4AA,H4AB), C7(H7BC,H7BD), C7(H7AA,H7AB), C8B(H8BA,H8BB),
 C3A(H3AA,H3AB)
4.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15)
4.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C10B(H10A,H10B,H10C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C10A(H10D,H10E,H10F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 142 electrons were 
found in a volume of 574\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 1.5[C7H8] per Formula Unit 
which account for 150 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              90378
_shelx_fab_checksum              12820
_olex2_submission_special_instructions 'No special instructions were received'