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_7717457
_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         'C35 H46 Br0.027 Mn N6.966 O2'
_chemical_formula_sum            'C35 H46 Br0.03 Mn N6.97 O2'
_chemical_formula_weight         653.47
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2024-04-17
_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                90
_cell_angle_beta                 90.347(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6595(7)
_cell_length_b                   9.0777(5)
_cell_length_c                   25.7615(13)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      22.47
_cell_measurement_theta_min      2.38
_cell_volume                     3662.0(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29267
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        22.533
_diffrn_reflns_theta_max         22.533
_diffrn_reflns_theta_min         1.526
_diffrn_source_current           0.99
_diffrn_source_power             0.0495
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.6704
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1214 before and 0.0541 after correction.
The Ratio of minimum to maximum transmission is 0.9001.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       blade
_exptl_crystal_F_000             1387
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.00059(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         4778
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0309P)^2^+1.8911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3777
_reflns_number_total             4778
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01765j3.cif
_cod_data_source_block           ts011_0m
_cod_depositor_comments
'Adding full bibliography for 7717456--7717459.cif.'
_cod_database_code               7717457
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.857
_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. Restrained distances
 Br2-Mn1
 2.55 with sigma of 0.01
3. Rigid bond restraints
 H3, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3, N2, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Rigid body (RIGU) restrains
 H3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, N2, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N1)=Sof(N2)=Sof(N3)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C15(H15), C13(H13), C14(H14), C19(H19)
6.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C21(H21A,H21B,H21C), C33(H33A,H33B,H33C), C27(H27A,H27B,H27C), C23(H23A,
 H23B,H23C), C34(H34A,H34B,H34C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              20804
_shelx_hkl_checksum              99639
_shelx_fab_checksum              46685
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'