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_7720261
_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         'C106.359 H130.696 N12 P4 Zn4, 1.663(C7 H8)'
_chemical_formula_sum            'C118 H144 N12 P4 Zn4'
_chemical_formula_weight         2115.80
_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   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2qlzkw
_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                100.505(2)
_cell_angle_beta                 99.090(2)
_cell_angle_gamma                100.839(2)
_cell_formula_units_Z            1
_cell_length_a                   11.8289(5)
_cell_length_b                   11.9812(5)
_cell_length_c                   20.7760(9)
_cell_measurement_reflns_used    7960
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      24.355
_cell_measurement_theta_min      2.699
_cell_volume                     2786.5(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      200.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            53749
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.467
_diffrn_reflns_theta_min         1.773
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0614 before and 0.0525 after correction.
The Ratio of minimum to maximum transmission is 0.8878.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       prism
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.780
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         11427
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0477
_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^)+(0.1021P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7692
_reflns_number_total             11427
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00139d2.cif
_cod_data_source_block           03733_0m
_cod_depositor_comments
'Adding full bibliography for 7720261--7720263.cif.'
_cod_database_code               7720261
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.856
_olex2_refinement_description
;
1. Rigid bond restraints
 Zn2, P2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
2. Uiso/Uaniso restraints and constraints
C53 \\sim C53A \\sim C54 \\sim C54A \\sim C55 \\sim C55A \\sim C56 \\sim C56A
\\sim C57 \\sim C57A \\sim C58 \\sim C58A \\sim C59 \\sim C59A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A
3. Others
 Sof(C53A)=Sof(H53D)=Sof(H53E)=Sof(H53F)=Sof(C54A)=Sof(C55A)=Sof(H55A)=
 Sof(C56A)=Sof(H56A)=Sof(C57A)=Sof(H57A)=Sof(C58A)=Sof(H58A)=Sof(C59A)=
 Sof(H59A)=1-FVAR(1)
 Sof(C54)=Sof(H54)=Sof(C55)=Sof(C56)=Sof(H56)=Sof(C57)=Sof(H57)=Sof(C58)=
 Sof(H58)=Sof(C59)=Sof(H59)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C50(H50), C24(H24), C21(H21), C47(H47)
4.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), C4(H4), C11(H11), C32(H32), C37(H37), C45(H45), C19(H19),
 C43(H43), C5(H5), C13(H13), C31(H31), C35(H35), C18(H18), C16(H16), C30(H30),
 C6(H6A), C7(H7), C36(H36), C33(H33), C9(H9), C44(H44), C17(H17), C12(H12),
 C10(H10), C39(H39), C38(H38), C15(H15), C41(H41), C42(H42), C54(H54), C56(H56),
  C57(H57), C58(H58), C59(H59), C55A(H55A), C56A(H56A), C57A(H57A), C58A(H58A),
 C59A(H59A)
4.c Fitted hexagon refined as free rotating group:
 C54(C55,C56,C57,C58,C59), C54A(C55A,C56A,C57A,C58A,C59A)
4.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C1(H1A,H1B,H1C), C49(H49A,H49B,H49C), C27(H27A,H27B,
 H27C), C52(H52A,H52B,H52C), C51(H51A,H51B,H51C), C22(H22A,H22B,H22C), C48(H48A,
 H48B,H48C), C25(H25A,H25B,H25C), C23(H23A,H23B,H23C), C53(H53A,H53B,H53C),
 C53A(H53D,H53E,H53F)
;
_shelx_res_checksum              21462
_shelx_hkl_checksum              59746
_olex2_submission_special_instructions 'No special instructions were received'