Crystal structure of a methyl benzoate quadruple-bonded dimolybdenum complex.
Bass, Lillian Dawson; Lee, Jessie H.; Lilygren, McKenzie C; Hartnett, Alaina C.; Campbell, Brandon M.; Morphet, Daniel R.; Dogutan, Dilek K.; Zheng, Shao-Liang; Acta crystallographica. Section E, Crystallographic communications 79 (2023) 231–235; doi:10.1107/S2056989023001457

data_2312071
_publ_section_title
;
 Crystal structure of a methyl benzoate quadruple-bonded dimolybdenum
 complex.
;
_journal_coeditor_code           EX2066
_journal_issue                   'Pt 3'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              231
_journal_page_last               235
_journal_paper_doi               10.1107/S2056989023001457
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          '[Mo2 (C8 H7 O2)4 (C4 H8 O)2], 2C4 H8 O'
_chemical_formula_moiety         'C40 H44 Mo2 O10, 2(C4 H8 O)'
_chemical_formula_sum            'C48 H60 Mo2 O12'
_chemical_formula_weight         1020.84
_chemical_name_systematic
'Tetrakis(\m-4-methylbenzoato-\k^2^<i>O</i>:<i>O</i>')[bis(tetrahydrofuran-\k<i>O</i>)molybdenum(II)] tetrahydrofuran disolvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                78.001(2)
_cell_angle_beta                 74.374(2)
_cell_angle_gamma                69.853(2)
_cell_formula_units_Z            1
_cell_length_a                   9.3923(7)
_cell_length_b                   10.6505(8)
_cell_length_c                   12.2955(9)
_cell_measurement_reflns_used    9495
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      2.36
_cell_volume                     1102.97(14)
_computing_cell_refinement
;
SAINT 8.37A (Bruker, 2015)
;
_computing_data_reduction
;
SAINT 8.37A (Bruker, 2015)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Bruker D8 goniometer with Photon 100 CMOS detector
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_source         'I\mS microfocus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22892
_diffrn_reflns_theta_full        25.087
_diffrn_reflns_theta_max         25.087
_diffrn_reflns_theta_min         2.365
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  0.7670
_exptl_absorpt_correction_T_min  0.7306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.652
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         3909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0302P)^2^+1.5476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0665
_reflns_number_gt                3693
_reflns_number_total             3909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ex2066sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1102.96(14)
_cod_database_code               2312071
_shelx_estimated_absorpt_t_min   0.873
_shelx_estimated_absorpt_t_max   0.917
_shelx_hkl_checksum              61888
_shelx_res_checksum              19885
_cod_database_fobs_code 2312071