Non-redox reactivity of V(II) and Fe(II) formamidinates towards CO2 resulting in the formation of novel M(II) carbamates
Korona, Krzesimir; Kornowicz, Arkadiusz; Justyniak, Iwona; Terlecki, Michał; Blachowski, Artur; Lewinski, Janusz; Dalton Transactions  (2022) –; doi:10.1039/D2DT02274E

data_7711482
_publ_section_title
;
 Non-redox reactivity of V(II) and Fe(II) formamidinates towards CO2
 resulting in the formation of novel M(II) carbamates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02274E
_journal_year                    2022
_chemical_formula_moiety         'C129 H176 Fe2 N10 O8, 2(C6 H14)'
_chemical_formula_sum            'C141 H204 Fe2 N10 O8'
_chemical_formula_weight         2278.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2022-09-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-09-29 deposited with the CCDC.	2022-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 92.430(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   21.550(5)
_cell_length_b                   29.745(5)
_cell_length_c                   22.858(5)
_cell_measurement_reflns_used    50407
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0340
_cell_measurement_theta_min      2.5250
_cell_volume                     14639(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics
;
CrystalMaker (Palmer, D. C. (2014) CrystalMaker Software Ltd, Begbroke, 
Oxfordshire, England.)
ORTEP III (Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.)
;
_computing_publication_material
;
Bourhis, L.J., Dolomanov, O.V., Gildea, R.J., Howard, J.A.K., Puschmann, H., 
(2015). Acta Cryst. A71, 59-75.
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H., 
J. Appl. Cryst. 42, 339-341.
;
_computing_structure_refinement
;
olex2.refine (Bourhis et al., 2015)
SHELXL (Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.)
;
_computing_structure_solution
'SHELXT (Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 16.2974
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.9980
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            256608
_diffrn_reflns_theta_full        26.4998
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.41
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale beige'
_exptl_crystal_density_diffrn    1.0340
_exptl_crystal_description       plate
_exptl_crystal_F_000             4948.6578
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.5997
_refine_diff_density_min         -0.6588
_refine_diff_density_rms         0.0757
_refine_ls_d_res_high            0.7964
_refine_ls_d_res_low             8.4507
_refine_ls_goodness_of_fit_ref   1.0676
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    312
_refine_ls_number_parameters     1494
_refine_ls_number_reflns         30281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0676
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.0079
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+15.5807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1356
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              19
_reflns_limit_h_min              -27
_reflns_limit_k_max              37
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              -18
_reflns_number_gt                22994
_reflns_number_total             30281
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt02274e2.cif
_cod_data_source_block           comp6(2)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7711482
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C20(H20), C23(H23), C33(H33), C36(H36), C46(H46), C49(H49),
 C59(H59), C62(H62), C72(H72), C75(H75), C85(H85), C88(H88), C98(H98),
 C101(H101), C111(H111), C114(H114), C124(H124), C127(H127)
2.b Secondary CH2 refined with riding coordinates:
 C145(H14d,H14e), C146(H14f,H14g), C147(H14h,H14i), C148(H14j,H14k), C151(H15d,
 H15e), C152(H15f,H15g), C153(H15h,H15i), C154(H15j,H15k)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C13(H13), C16(H16), C17(H17), C18(H18), C29(H29),
 C30(H30), C31(H31), C39(H39), C42(H42), C43(H43), C44(H44), C55(H55), C56(H56),
  C57(H57), C65(H65), C68(H68), C69(H69), C70(H70), C81(H81), C82(H82),
 C83(H83), C91(H91), C94(H94), C95(H95), C96(H96), C107(H107), C108(H108),
 C109(H109), C117(H117), C120(H120), C121(H121), C122(H122), N2(H2)
2.d Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c),
 C21(H21a,H21b,H21c), C22(H22a,H22b,H22c), C24(H24a,H24b,H24c), C25(H25a,H25b,
 H25c), C34(H34a,H34b,H34c), C35(H35a,H35b,H35c), C37(H37a,H37b,H37c), C38(H38a,
 H38b,H38c), C47(H47a,H47b,H47c), C48(H48a,H48b,H48c), C50(H50a,H50b,H50c),
 C51(H51a,H51b,H51c), C60(H60a,H60b,H60c), C61(H61a,H61b,H61c), C63(H63a,H63b,
 H63c), C64(H64a,H64b,H64c), C73(H73a,H73b,H73c), C74(H74a,H74b,H74c), C76(H76a,
 H76b,H76c), C77(H77a,H77b,H77c), C86(H86a,H86b,H86c), C87(H87a,H87b,H87c),
 C89(H89a,H89b,H89c), C90(H90a,H90b,H90c), C99(H99a,H99b,H99c), C100(H10a,H10b,
 H10c), C102(H10d,H10e,H10f), C103(H10g,H10h,H10i), C112(H11d,H11e,H11f),
 C113(H11g,H11h,H11i), C115(H11j,H11k,H11l), C116(H11m,H11n,H11o), C125(H12d,
 H12e,H12f), C126(H12g,H12h,H12i), C128(H12j,H12k,H12l), C129(H12m,H12n,H12o),
 C144(H14a,H14b,H14c), C149(H14l,H14m,H14n), C150(H15a,H15b,H15c), C155(H15l,
 H15m,H15n)
FREE comand was used to removed the connectivity bond Fe1-C104 from the list.
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 382 electrons were found in a volume of 2349 A 
per unit cell. This is consistent with the presence of 4 C6H14 per Unit Cell 
account for 382 electrons.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'