Exploiting decarbonylation and dehydrogenation of formamides for the synthesis of ureas, polyureas, and poly(urea-urethanes).
Luk, James; Goodfellow, Alister S.; More, Nachiket Deepak; Bühl, Michael; Kumar, Amit; Chemical science 15 (2024) 16594–16604; doi:10.1039/d4sc03948c

data_1572509
_publ_section_title
;
 Exploiting decarbonylation and dehydrogenation of formamides for the
 synthesis of ureas, polyureas, and poly(urea-urethanes).
;
_journal_issue                   40
_journal_name_full               'Chemical science'
_journal_page_first              16594
_journal_page_last               16604
_journal_paper_doi               10.1039/d4sc03948c
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C37 H38 N2 O2 P2 Ru, C8 H9 N O'
_chemical_formula_sum            'C45 H47 N3 O3 P2 Ru'
_chemical_formula_weight         840.86
_chemical_name_systematic
'carbonyl-hydrido-(bis(2-(diphenylphosphino)ethyl)amine)-(N-benzylformamide)-ruthenium N-benzylformamide'
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-05-17 deposited with the CCDC.	2024-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                85.247(2)
_cell_angle_beta                 80.723(2)
_cell_angle_gamma                85.7580(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3385(2)
_cell_length_b                   12.9630(2)
_cell_length_c                   15.3995(4)
_cell_measurement_reflns_used    14159
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.4190
_cell_measurement_theta_min      1.5610
_cell_volume                     2025.95(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.841
_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    -85.00  93.00   0.50   42.00    --    4.40  45.00 178.65  356
  2  \w     57.00  93.00   0.50   42.00    --    4.40  45.00   0.00   72
  3  \w     39.00  78.00   0.50   42.00    --  -10.90  45.00 150.00   78
  4  \w     33.00  73.00   0.50   42.00    --  -10.90  45.00  30.00   80
  5  \w     23.00  64.00   0.50   42.00    --  -10.90  45.00  90.00   82
  6  \w   -100.00  19.00   0.50   42.00    --  -10.90  45.00  30.00  238
  7  \w   -100.00 -52.00   0.50   42.00    --  -10.90  45.00 150.00   96
  8  \w    -75.00 -49.00   0.50   42.00    --  -10.90  45.00  60.00   52
  9  \w     -2.00  63.00   0.50   42.00    --  -10.90  45.00  60.00  130
 10  \w    -95.00 -69.00   0.50   42.00    --  -10.90  45.00 120.00   52
 11  \w    -66.00 -31.00   0.50   42.00    --  -10.90  45.00 120.00   70
 12  \w     53.00  78.00   0.50   42.00    --  -10.90  45.00 120.00   50
 13  \w   -100.00  78.00   0.50   42.00    --  -10.90  45.00 -16.62  356
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0047409000
_diffrn_orient_matrix_UB_12      -0.0032093000
_diffrn_orient_matrix_UB_13      -0.0461744000
_diffrn_orient_matrix_UB_21      -0.0342690000
_diffrn_orient_matrix_UB_22      -0.0461262000
_diffrn_orient_matrix_UB_23      0.0075606000
_diffrn_orient_matrix_UB_31      -0.0604499000
_diffrn_orient_matrix_UB_32      0.0298032000
_diffrn_orient_matrix_UB_33      0.0005052000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44155
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.456
_diffrn_reflns_theta_min         1.579
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
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    1.378
_exptl_crystal_description       needle
_exptl_crystal_F_000             872
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         9459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0358P)^2^+0.7138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7401
_reflns_number_total             9459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03948c2.cif
_cod_data_source_block           jlak2
_cod_depositor_comments
'Adding full bibliography for 1572508--1572509.cif.'
_cod_database_code               1572509
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C36 H35 N2 O2 P2 Ru'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C30(H30A,H30B), C5(H5A,H5B), C38(H38A,
 H38B)
2.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C7(H7), C37(H37), C8(H8), C13(H13), C11(H11), C36(H36), C35(H35),
 C32(H32), C29(H29), C26(H26), C28(H28), C27(H27), C19(H19), C23(H23), C16(H16),
  C15(H15), C9(H9), C17(H17), C34(H34), C33(H33), C25(H25), C14(H14), C21(H21),
 C10(H10), C22(H22), C20(H20), C43(H43), C40(H40), C44(H44), C42(H42), C41(H41),
  C45(H45)
;
_shelx_res_checksum              43344
_shelx_hkl_checksum              28899
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.345
_oxdiff_exptl_absorpt_empirical_full_min 0.729