Crystal structure of a trifluoromethyl benzoato quadruple-bonded dimolybdenum complex
Aigeldinger, Elisabeth; Brandao, Lilliana; Powell, Troy; Hartnett, Alaina C.; Sun, Rui; Dogutan, Dilek K.; Zheng, Shao-Liang; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S205698902200010X

data_2243996
_publ_section_title
;
 Crystal structure of a trifluoromethyl benzoato quadruple-bonded
 dimolybdenum complex
;
_journal_coeditor_code           MW2183
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205698902200010X
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac
'[Mo2 (C8 H4 F3 O2)4 (C4 H8 O)2] , 0.762 C5 H12 , 0.238 C4 H8 O'
_chemical_formula_moiety
'C40 H32 F12 Mo2 O10, 0.238(C4 H8 O), 0.762(C5 H12)'
_chemical_formula_sum            'C44.76 H43.05 F12 Mo2 O10.24'
_chemical_formula_weight         1164.68
_chemical_name_systematic
;
Tetrakis(\m-4-trifluoromethylbenzoato-\k^2^<i>O</i>:<i>O</i>')dimolybdenum(II)
0.762-pentane 0.238-tetrahydrofuran solvate
;
_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                85.843(13)
_cell_angle_beta                 81.208(8)
_cell_angle_gamma                83.107(16)
_cell_formula_units_Z            1
_cell_length_a                   7.7687(17)
_cell_length_b                   12.099(5)
_cell_length_c                   12.572(2)
_cell_measurement_reflns_used    9835
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      2.48
_cell_volume                     1157.6(6)
_computing_cell_refinement
;
SAINT  (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008), and PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0326
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            39433
_diffrn_reflns_theta_full        25.097
_diffrn_reflns_theta_max         25.097
_diffrn_reflns_theta_min         2.669
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7011
_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    1.671
_exptl_crystal_description       block
_exptl_crystal_F_000             586
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.394
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         4094
_refine_ls_number_restraints     713
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+2.0296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0640
_reflns_number_gt                3814
_reflns_number_total             4094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mw2183sup1.cif
_cod_data_source_block           I
_cod_database_code               2243996
_shelx_estimated_absorpt_t_min   0.831
_shelx_estimated_absorpt_t_max   0.965
_shelx_hkl_checksum              92774
_shelx_res_checksum              4871
_cod_database_fobs_code 2243996