Investigating the formation of metal nitride complexes employing a tetradentate bis-carbene bis-phenolate ligand.
Kunert, Romain; Martelino, Diego; Mahato, Samyadeb; Hein, Nicholas M.; Pulfer, Jason; Philouze, Christian; Jarjayes, Olivier; Thomas, Fabrice; Storr, Tim; Dalton transactions (Cambridge, England : 2003) 54 (2025) 616–630; doi:10.1039/d4dt01765j

data_7717458
_publ_section_title
;
 Investigating the formation of metal nitride complexes employing a
 tetradentate bis-carbene bis-phenolate ligand.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              616
_journal_page_last               630
_journal_paper_doi               10.1039/d4dt01765j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'Cl, C35 H48 N5 O2, H2 O, 0.748(C1 H2 Cl2), 1.25(C2 H3 N)'
_chemical_formula_sum            'C38.25 H55.24 Cl2.5 N6.25 O3'
_chemical_formula_weight         739.08
_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
_audit_creation_date             2024-05-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2024-05-30 deposited with the CCDC.	2024-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                96.27(3)
_cell_angle_beta                 96.47(3)
_cell_angle_gamma                106.01(3)
_cell_formula_units_Z            2
_cell_length_a                   8.1811(16)
_cell_length_b                   13.290(3)
_cell_length_c                   20.518(4)
_cell_measurement_reflns_used    33145
_cell_measurement_temperature    210
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      2.392
_cell_volume                     2107.6(9)
_computing_cell_refinement       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT-2016 (Sheldrick, 2008)'
_diffrn_ambient_temperature      210.00
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '\k-geometry 4 circles diffractometer'
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaAPEXII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33145
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.392
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.513887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1274 before and 0.0773 after correction.
The Ratio of minimum to maximum transmission is 0.5139.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       prism
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         7349
_refine_ls_number_restraints     244
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0642
_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^)+(0.0814P)^2^+1.4610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1592
_refine_ls_wR_factor_ref         0.1818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5498
_reflns_number_total             7349
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01765j3.cif
_cod_data_source_block           sad
_cod_depositor_comments
'Adding full bibliography for 7717456--7717459.cif.'
_cod_original_cell_volume        2107.6(8)
_cod_original_formula_sum        'C38.25 H55.24 Cl2.50 N6.25 O3'
_cod_database_code               7717458
_shelx_shelxl_version_number     2019/3
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C38B-Cl2B
 1.7 with sigma of 0.02
 C38B-Cl3B
 1.7 with sigma of 0.02
 Cl3A-C38A
 1.7 with sigma of 0.02
 C38A-Cl2A
 1.7 with sigma of 0.02
 C37A-C36A
 1.5 with sigma of 0.02
 C36B-C37B
 1.5 with sigma of 0.02
 N6A-C36A
 1.1 with sigma of 0.02
 N6B-C36B
 1.1 with sigma of 0.02
 N6A-C37A
 2.7 with sigma of 0.02
 C37B-N6B
 2.7 with sigma of 0.02
 C38C-N7C
 1.2 with sigma of 0.02
 C39C-C38C
 1.5 with sigma of 0.02
 C39C-N7C
 2.7 with sigma of 0.02
3. Rigid bond restraints
 Cl3B, Cl2B, C38B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl3B, Cl3A, C38B, C38A, Cl2B, Cl2A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C32, C33B, C35B, C34B, C34, C33, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C36A, C37A, N6A, C36B, C37B, N6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C39C, C38C, N7C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl3B \\sim Cl2B \\sim C38B: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
Cl3B \\sim Cl3A \\sim C38B \\sim C38A \\sim Cl2B \\sim Cl2A: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
C32 \\sim C33B \\sim C35B \\sim C34B \\sim C34 \\sim C33 \\sim C35: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
C36B \\sim C37A \\sim C36A \\sim N6A \\sim C37B \\sim N6B: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
C39C \\sim C38C \\sim N7C: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 1.7A
Uanis(C37A) \\sim Ueq, Uanis(C37B) \\sim Ueq, Uanis(C36A) \\sim Ueq,
Uanis(C36B) \\sim Ueq, Uanis(N6B) \\sim Ueq, Uanis(N6A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C34)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C33)=Sof(H33D)=Sof(H33E)=Sof(H33F)=
 Sof(C35)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(1)
 Sof(C33B)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C35B)=Sof(H35A)=Sof(H35B)=
 Sof(H35C)=Sof(C34B)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Sof(Cl3B)=Sof(Cl2B)=Sof(C38B)=Sof(H38A)=Sof(H38B)=FVAR(2)
 Sof(C36B)=Sof(C37B)=Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(N6B)=1-FVAR(3)
 Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C36A)=Sof(N6A)=FVAR(3)
 Sof(Cl3A)=Sof(Cl2A)=Sof(C38A)=Sof(H38C)=Sof(H38D)=FVAR(4)
 Fixed Sof: C38C(0.25) N7C(0.25) C39C(0.25) H39A(0.25) H39B(0.25) H39C(0.25)
6.a Free rotating group:
 O1(H1), O2(H2), O3(H3A,H3B)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C38B(H38A,H38B), C38A(H38C,H38D)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C8(H8), C4(H4), C12(H12), C14(H14), C18(H18), C19(H19), C9(H9)
6.d Idealised Me refined with riding coordinates:
 C37A(H37A,H37B,H37C), C37B(H37D,H37E,H37F)
6.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C31(H31A,H31B,H31C), C27(H27A,H27B,H27C), C21(H21A,H21B,H21C), C30(H30A,
 H30B,H30C), C29(H29A,H29B,H29C), C33B(H33A,H33B,H33C), C35B(H35A,H35B,H35C),
 C34B(H34A,H34B,H34C), C34(H34D,H34E,H34F), C33(H33D,H33E,H33F), C35(H35D,H35E,
 H35F), C39C(H39A,H39B,H39C)
;
_shelx_res_checksum              83135
_shelx_hkl_checksum              28133
_olex2_submission_special_instructions 'No special instructions were received'