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_7717456
_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 Br Mn N4 O2'
_chemical_formula_sum            'C35 H46 Br Mn N4 O2'
_chemical_formula_weight         689.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-04-16
_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                 122.3273(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.477(2)
_cell_length_b                   15.0603(11)
_cell_length_c                   20.2126(14)
_cell_measurement_reflns_used    9616
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.62
_cell_measurement_theta_min      2.21
_cell_volume                     7839.5(10)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker D8 diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            165068
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.737
_diffrn_reflns_theta_min         1.581
_exptl_absorpt_coefficient_mu    1.387
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0553 before and 0.0495 after correction. The Ratio of minimum to maximum transmission is 0.9320. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       needle
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.399
_refine_diff_density_min         -1.555
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         10145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+14.4826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7774
_reflns_number_total             10145
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01765j3.cif
_cod_data_source_block           ts006
_cod_depositor_comments
'Adding full bibliography for 7717456--7717459.cif.'
_cod_database_code               7717456
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.338
_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.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C15(H15), C14(H14), C18(H18), C19(H19), C5(H5), C3(H3)
2.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C35(H35A,H35B,H35C), C33(H33A,H33B,H33C), C21(H21A,
 H21B,H21C), C23(H23A,H23B,H23C), C34(H34A,H34B,H34C), C22(H22A,H22B,H22C),
 C27(H27A,H27B,H27C)
;
_shelx_res_checksum              27862
_shelx_hkl_checksum              26242
_shelx_fab_checksum              2800
_olex2_submission_special_instructions 'No special instructions were received'