Efficient synthesis of cyclic carbonates and oxazolidinones by simple zinc guanidinato complexes.
Ginés, Carlos; Parra-Cadenas, Blanca; Elorriaga, David; García-Vivó, Daniel; Fernández-Galán, Rafael; Ramos, Alberto; Carrillo-Hermosilla, Fernando; Dalton transactions (Cambridge, England : 2003) 55 (2026) 4525–4534; doi:10.1039/d6dt00139d

data_7720262
_publ_section_title
;
 Efficient synthesis of cyclic carbonates and oxazolidinones by simple
 zinc guanidinato complexes.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4525
_journal_page_last               4534
_journal_paper_doi               10.1039/d6dt00139d
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C40 H54 N6 S2 Zn2'
_chemical_formula_sum            'C40 H54 N6 S2 Zn2'
_chemical_formula_weight         813.75
_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
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2qlzlx
_audit_creation_date             2025-11-27
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-01-06 deposited with the CCDC.	2026-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.101(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0842(5)
_cell_length_b                   34.2298(10)
_cell_length_c                   11.1316(4)
_cell_measurement_reflns_used    21770
_cell_measurement_temperature    250.00(14)
_cell_measurement_theta_max      28.7640
_cell_measurement_theta_min      2.3560
_cell_volume                     4134.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      250.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.824
_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    -76.00   4.00   0.50   20.00    --   -3.06 -19.00-120.00  160
  2  \w    -75.00  10.00   0.50   20.00    --   -3.06 -57.00  30.00  170
  3  \w    -23.00  33.00   0.50   20.00    --    3.14 -99.00 -30.00  112
  4  \w    -23.00  33.00   0.50   20.00    --    3.14 -99.00-180.00  112
  5  \w    -23.00   3.00   0.50   20.00    --    3.14 -99.00  90.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.824
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            48378
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.824
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.042
_diffrn_reflns_theta_min         2.122
_exptl_absorpt_coefficient_mu    1.296
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.476
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       plate
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         10900
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0411P)^2^+7.6467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8869
_reflns_number_total             10900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00139d2.cif
_cod_data_source_block           03777
_cod_depositor_comments
'Adding full bibliography for 7720261--7720263.cif.'
_cod_database_code               7720262
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.660
_olex2_refinement_description
;
1. Restrained distances
 C18-C19 = C18A-C19A = C36-C37 = C36A-C37A = C39-C40 = C39A-C40A
 2.45 with sigma of 0.04
 C18-C19 \\sim C18A-C19A \\sim C18-C20 \\sim C18A-C20A \\sim N2-C18 \\sim
N2-C18A \\sim C35-C36 \\sim C35-
 C36A \\sim C35-C37 \\sim C35-C37A \\sim C38-C39 \\sim C38-C39A \\sim C38-C40
\\sim C38-C40A
 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
C18 \\sim C18A \\sim C19 \\sim C19A \\sim C20 \\sim C20A \\sim C37 \\sim C37A
\\sim C36 \\sim C36A \\sim C39 \\sim C39A \\sim C40 \\sim C40A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
3. Others
 Sof(H38A)=Sof(H35A)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20A)=
 Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C18A)=Sof(H18A)=Sof(C36A)=Sof(H36D)=
 Sof(H36E)=Sof(H36F)=Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C39A)=
 Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(1)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C18)=Sof(H18)=Sof(H38)=Sof(H35)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C18(H18), C38(H38A), C38(H38), C35(H35), C35(H35A), C15(H15), C18A(H18A)
4.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), C24(H24), C4(H4), C33(H33), C6(H6A), C12(H12), C31(H31),
 C26(H26), C7(H7), C11(H11), C3(H3A), C30(H30), C32(H32), C10(H10), C23(H23),
 C25(H25), C13(H13), C5(H5), C27(H27)
4.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C16(H16A,H16B,H16C), C37(H37A,H37B,
 H37C), C21(H21A,H21B,H21C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C17(H17A,
 H17B,H17C), C1(H1A,H1B,H1C), C36(H36A,H36B,H36C), C19A(H19D,H19E,H19F),
 C20A(H20D,H20E,H20F), C36A(H36D,H36E,H36F), C37A(H37D,H37E,H37F), C39A(H39D,
 H39E,H39F), C40A(H40D,H40E,H40F)
;
_shelx_res_checksum              8265
_shelx_hkl_checksum              65858
_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
;