Untangling ancillary ligand donation <i>versus</i> locus of oxidation effects on metal nitride reactivity.
Mahato, Samyadeb; VandeVen, Warren; MacNeil, Gregory A.; Pulfer, Jason M.; Storr, Tim; Chemical science 15 (2024) 2211–2220; doi:10.1039/d3sc05403a

data_1570619
_publ_section_title
;
 Untangling ancillary ligand donation <i>versus</i> locus of oxidation
 effects on metal nitride reactivity.
;
_journal_issue                   6
_journal_name_full               'Chemical science'
_journal_page_first              2211
_journal_page_last               2220
_journal_paper_doi               10.1039/d3sc05403a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         '0.121(C28 H36 Mn N3 O2)'
_chemical_formula_sum            'C3.39 H4.36 Mn0.12 N0.36 O0.24'
_chemical_formula_weight         60.79
_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_date             2023-04-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-09-29 deposited with the CCDC.	2024-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.227(13)
_cell_angle_gamma                90
_cell_formula_units_Z            33
_cell_length_a                   13.155(3)
_cell_length_b                   12.7828(10)
_cell_length_c                   15.378(2)
_cell_measurement_reflns_used    9825
_cell_measurement_temperature    298.14
_cell_measurement_theta_max      63.915
_cell_measurement_theta_min      4.526
_cell_volume                     2544.8(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.14
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker PHOTON II 14 CPAD'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32249
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        64.797
_diffrn_reflns_theta_max         64.797
_diffrn_reflns_theta_min         4.528
_diffrn_source_current           0.65
_diffrn_source_power             0.02925
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    4.443
_exptl_absorpt_correction_T_max  0.7525
_exptl_absorpt_correction_T_min  0.5703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1449 before and 0.0699 after correction.
The Ratio of minimum to maximum transmission is 0.7579.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          1.146
_exptl_crystal_size_mid          0.304
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         4226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0465P)^2^+0.6086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3592
_reflns_number_total             4226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05403a2.cif
_cod_data_source_block           cu_ts_smsample1_0m_a
_cod_depositor_comments          'Adding full bibliography for 1570619.cif.'
_cod_database_code               1570619
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.456
_shelx_estimated_absorpt_t_min   0.080
_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 Ternary CH refined with riding coordinates:
 C00J(H00J), C00M(H00M)
2.b Secondary CH2 refined with riding coordinates:
 C00O(H00A,H00B), C00Q(H00C,H00D), C00U(H00W,H00X), C00X(H00,HD)
2.c Aromatic/amide H refined with riding coordinates:
 C009(H009), C00E(H00E), C00F(H00F), C00G(H00G), C00I(H00I), C00K(H00K),
 C00L(H00L), C00P(H00P)
2.d Idealised Me refined as rotating group:
 C00R(H00H,H00N,H00O), C00S(H00Q,H00R,H00S), C00T(H00T,H00U,H00V), C00V(H00Y,H,
 HA), C00W(H00Z,HB,HC), C00Y(H1,HE,HF)
;
_shelx_res_checksum              20807
_shelx_hkl_checksum              12373
_olex2_exptl_crystal_mounting_method 'Mounted in Parabar oil'
_olex2_submission_special_instructions 'No special instructions were received'