Exploring early transition metal coordination: a synthetic and computational study of tripodal ligand complexes.
Moore, Jewelianna M.; Vaught, Brennan M.; Miller, Tabitha J.; Nunn, George; Elford, Lindsey S.; Gullett, Kelly L.; Walton, Paul H.; Fout, Alison R.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 16177–16182; doi:10.1039/d5dt01888a

data_7719673
_publ_section_title
;
 Exploring early transition metal coordination: a synthetic and
 computational study of tripodal ligand complexes.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16177
_journal_page_last               16182
_journal_paper_doi               10.1039/d5dt01888a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C36 H48 Mo N7'
_chemical_formula_sum            'C36 H48 Mo N7'
_chemical_formula_weight         674.75
_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
_atom_sites_solution_primary     'dual space'
_audit_creation_date             2025-06-04
_audit_creation_method
; 
Olex2 1.5 
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254) 
;
_audit_update_record
;
2025-08-07 deposited with the CCDC.	2025-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.3340(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7803(5)
_cell_length_b                   20.8514(9)
_cell_length_c                   14.1302(6)
_cell_measurement_reflns_used    9608
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.43
_cell_volume                     3162.5(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX3 V2018.7-2 (Bruker, 2018)'
_computing_data_reduction
; 
SAINT V8.38A, XPREP v2014/2, (Bruker, 2018), SADABS V2016/2 
(Krause et al., 2015) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-7 (Bruker, 2018), CrystalMaker v9.2.8 (CrystalMaker, 2016) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2018)'
_computing_structure_refinement  'SHELXL-2018-3 (Sheldrick, 2015a)'
_computing_structure_solution    'SHELXT-2014-5 (Sheldrick, 2015b)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker D8 Venture/Photon II'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ed22fs
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            71092
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.379
_diffrn_reflns_theta_min         2.431
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Krause et al., 2015)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1420
_exptl_crystal_id                ed22fs
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Paratone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-1 -4 4) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.059
_refine_diff_density_max         1.220
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0431P)^2^+5.8968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5952
_reflns_number_total             6462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01888a2.cif
_cod_data_source_block           ed22fs
_cod_depositor_comments
'Adding full bibliography for 7719670--7719673.cif.'
_cod_database_code               7719673
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.900
_exptl_absorpt_special_details   none
_olex2_refinement_description
; 
1.a Ternary CH refined with riding coordinates: 
 C15(H15), C27(H27), C39(H39) 
1.b Secondary CH2 refined with riding coordinates: 
 C17(H17A,H17B), C16(H16A,H16B), C9(H9A,H9B), C19(H19A,H19B), C21(H21A,H21B), 
 C18(H18A,H18B), C20(H20A,H20B), C31(H31A,H31B), C33(H33A,H33B), 
C32(H32A,H32B), 
  C29(H29A,H29B), C30(H30A,H30B), C42(H42A,H42B), C28(H28A,H28B), C44(H44A, 
 H44B), C40(H40A,H40B), C43(H43A,H43B), C41(H41A,H41B) 
1.c Aromatic/amide H refined with riding coordinates: 
 C14(H14), C11(H11), C35(H35), C23(H23), C24(H24), C36(H36), C26(H26), 
 C12(H12), C38(H38) 
;
_shelx_res_checksum              14839
_shelx_hkl_checksum              62647
_olex2_submission_original_sample_id ed22fs
_olex2_submission_special_instructions
;
No special instructions were received
;