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_7719670
_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 Cr N7'
_chemical_formula_sum            'C36 H48 Cr N7'
_chemical_formula_weight         630.81
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_audit_creation_date             2023-08-14
_audit_creation_method
; 
Olex2 1.5 
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) 
;
_audit_update_record
;
2025-08-07 deposited with the CCDC.	2025-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.520(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5541(4)
_cell_length_b                   20.8052(7)
_cell_length_c                   14.3671(6)
_cell_measurement_reflns_used    9032
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.17
_cell_volume                     3140.1(2)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_data_reduction
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2014/7, (Bruker, 2014) 
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELX-2014-7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-2014-7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  13
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            84608
_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         25.371
_diffrn_reflns_theta_min         1.958
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016) was used for absorption correction. 
wR2(int) was 0.0667 before and 0.0590 after correction. 
The Ratio of minimum to maximum transmission is 0.9612. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       trianglar
_exptl_crystal_F_000             1348
_exptl_crystal_id                13
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the 0 -1 -1 scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0453P)^2^+5.2422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5365
_reflns_number_total             5767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01888a2.cif
_cod_data_source_block           13
_cod_depositor_comments
'Adding full bibliography for 7719670--7719673.cif.'
_cod_database_code               7719670
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.940
_olex2_refinement_description
; 
1.a Ternary CH refined with riding coordinates: 
 C19(H19), C25(H25), C31(H31) 
1.b Secondary CH2 refined with riding coordinates: 
 C1(H1A,H1B), C7(H7A,H7B), C13(H13A,H13B), C20(H20A,H20B), C21(H21A,H21B), 
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B), 
C27(H27A,H27B), 
  C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A, 
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B) 
1.c Aromatic/amide H refined with riding coordinates: 
 C3(H3), C4(H4), C6(H6), C9(H9), C10(H10), C12(H12), C15(H15), C16(H16), 
 C18(H18) 
;
_olex2_submission_original_sample_id 13
_olex2_submission_special_instructions 'No special instructions were received'