Crystal structures of two dioxomolybdenum complexes stabilized by salan ligands featuring phenyl and cyclohexyl backbones
Trieu-Tran, Tristhan; Martinez, Stephenie N.; Brannon, Jacob P.; Stieber, S. Chantal E.; John, Alex; Acta Crystallographica Section E Crystallographic Communications 78 (2022) –; doi:10.1107/S2056989022000524

data_2022532
_publ_section_title
;
 Crystal structures of two dioxomolybdenum complexes stabilized by salan
 ligands featuring phenyl and cyclohexyl backbones
;
_journal_coeditor_code           TX2046
_journal_issue                   3
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989022000524
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          '[Mo (C36 H56 N2 O2) O2], 2C H4 O'
_chemical_formula_moiety         'C36 H56 Mo N2 O4, 2(C H4 O)'
_chemical_formula_sum            'C38 H64 Mo N2 O6'
_chemical_formula_weight         740.84
_chemical_name_systematic
;(6,6'-{[(Cyclohexane-1,2-diyl)bis(azanediyl)]bis(methylene)}bis(2,4-di-<i>tert</i>-butylphenolato))dioxidomolybdenum(VI)
methanol disolvate
;
_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_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.035(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4889(14)
_cell_length_b                   10.9722(8)
_cell_length_c                   19.1517(14)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      51.42
_cell_measurement_theta_min      5.28
_cell_volume                     3875.6(5)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015)
;
_diffrn_ambient_temperature      105.32
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29075
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         5.282
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.383
_exptl_absorpt_correction_T_max  0.7503
_exptl_absorpt_correction_T_min  0.6718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       prism
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.520
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         9532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0277P)^2^+2.9594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0702
_reflns_number_gt                8724
_reflns_number_total             9532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tx2046sup1.cif
_cod_data_source_block           2b
_cod_original_formula_sum        'C38 H64 Mo1 N2 O6'
_cod_database_code               2022532
_shelx_estimated_absorpt_t_min   0.927
_shelx_estimated_absorpt_t_max   0.963
_shelx_hkl_checksum              28395
_shelx_res_checksum              69038
_cod_database_fobs_code 2022532