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_7711477
_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         'C54 H78 N4 O V'
_chemical_formula_sum            'C54 H78 N4 O V'
_chemical_formula_weight         850.19
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-22
_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
_cell_angle_beta                 107.502(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2867(3)
_cell_length_b                   14.7719(2)
_cell_length_c                   25.4469(4)
_cell_measurement_reflns_used    17273
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.8950
_cell_measurement_theta_min      2.2860
_cell_volume                     5480.24(17)
_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  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 16.2974
_diffrn_measured_fraction_theta_full 0.9967
_diffrn_measured_fraction_theta_max 0.9967
_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  0.0257
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            49808
_diffrn_reflns_theta_full        26.4973
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.17
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.0304
_exptl_crystal_description       plate
_exptl_crystal_F_000             1845.8810
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.5517
_refine_diff_density_min         -0.3107
_refine_diff_density_rms         0.0542
_refine_ls_d_res_high            0.7965
_refine_ls_d_res_low             9.3765
_refine_ls_goodness_of_fit_ref   0.8625
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    120
_refine_ls_number_parameters     557
_refine_ls_number_reflns         11308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.8625
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+3.4987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1218
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -19
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              -13
_reflns_number_gt                9702
_reflns_number_total             11308
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt02274e2.cif
_cod_data_source_block           comp2
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               7711477
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C60(0.5) H60a(0.5) H60b(0.5) H60c(0.5) C61(0.5) H61a(0.5)
 H61b(0.5) C62(0.5) H62a(0.5) H62b(0.5) C63(0.5) H63a(0.5) H63b(0.5) C64(0.5)
 H64a(0.5) H64b(0.5) H64c(0.5)
3.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C24(H24), C27(H27), C36(H36), C39(H39), C49(H49), C52(H52)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b)
3.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C17(H17), C20(H20), C21(H21), C22(H22), C32(H32),
 C33(H33), C34(H34), C42(H42), C45(H45), C46(H46), C47(H47)
3.d Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C13(H13a,H13b,H13c), C15(H15a,H15b,H15c), C16(H16a,H16b,
 H16c), C25(H25a,H25b,H25c), C26(H26a,H26b,H26c), C28(H28a,H28b,H28c), C29(H29a,
 H29b,H29c), C37(H37a,H37b,H37c), C38(H38a,H38b,H38c), C40(H40a,H40b,H40c),
 C41(H41a,H41b,H41c), C50(H50a,H50b,H50c), C51(H51a,H51b,H51c), C53(H53a,H53b,
 H53c), C54(H54a,H54b,H54c)
FREE comand was used to removed the connectivity bonds V1 C17 and V1 C42 from the list.
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 130 electrons were 
found in a volume of 1051 A in 2 voids per unit cell. 
This is consistent with the presence of 
1.5[C5H12] per Unit Cell which account for 130 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'