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_7711481
_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_sum            'C221 H304 Fe4 N16 O14'
_chemical_formula_weight         3632.18
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2022-09-29 deposited with the CCDC.	2022-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.0129(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.00932(15)
_cell_length_b                   64.6462(8)
_cell_length_c                   25.1469(3)
_cell_measurement_reflns_used    31346
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0970
_cell_measurement_theta_min      2.3320
_cell_volume                     22760.2(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
;
WinGX: Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.)
Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., OLEX2: 
(2009). J. Appl. Cryst., 42, 339-341
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2974
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.889
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -85
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            96823
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.249
_diffrn_reflns_theta_min         2.350
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.953
_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    1.060
_exptl_crystal_description       block
_exptl_crystal_F_000             7832
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2387
_refine_ls_number_reflns         50059
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+42.1718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1490
_reflns_Friedel_coverage         0.000
_reflns_number_gt                38802
_reflns_number_total             50059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02274e2.cif
_cod_data_source_block           shelx_CCDC3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7711481
_shelx_shelxl_version_number     2016/6
_smtbx_masks_special_details
;
A solvent mask was calculated and 524 electrons were 
found in a volume of 3492\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[C6H14], 1.5[C6H14] per Unit Cell 
which account for 500 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              71215
_shelx_fab_checksum              6752