Hydrothermal Synthesis and Structure of a Dinuclear Molybdenum(III) Hydroxy Squarate with a Mo‒Mo Bond
Barber, Greg D.; George, Christy; Hogg, Kathryn; Johnstone, Shae T.; Pacheco, Carlos N.; Yennawar, Hemant P.; Van Der Sluys, William G.; ACS Omega  (2020) –; doi:10.1021/acsomega.0c00083

data_4517451
_publ_section_title
;
 Hydrothermal Synthesis and Structure of a Dinuclear Molybdenum(III)
 Hydroxy Squarate with a Mo--Mo Bond
;
_journal_name_full               'ACS Omega'
_journal_paper_doi               10.1021/acsomega.0c00083
_journal_year                    2020
_chemical_formula_moiety         'C4 H3 Mo O7, H2 O'
_chemical_formula_sum            'C4 H5 Mo O8'
_chemical_formula_weight         277.02
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-02-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                105.747(18)
_cell_angle_beta                 96.866(19)
_cell_angle_gamma                115.116(17)
_cell_formula_units_Z            2
_cell_length_a                   7.555(9)
_cell_length_b                   7.727(9)
_cell_length_c                   8.337(9)
_cell_measurement_reflns_used    2174
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.222
_cell_measurement_theta_min      2.643
_cell_volume                     408.5(8)
_computing_cell_refinement       'SAINT V6.36A (BRUKER, 2001)'
_computing_data_collection       'SMART V5.634 (Bruker Inc., 2001)'
_computing_data_reduction        'SAINT V6.36A (BRUKER, 2001)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 8.34
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3706
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.64
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           32.0
_diffrn_source_power             1600
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.620
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.218588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS V2.05 (BRUKER, 2001) was used for absorption correction. R(int) was 0.0298 before 
and 0.0036 after correction. The Ratio of minimum to maximum transmission is 0.2186. 
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             270
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.992
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+1.1857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                1798
_reflns_number_total             1890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ao0c00083_si_002.cif
_cod_data_source_block           wgv3s
_cod_database_code               4517451
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O8(H8A,H8B)
2.b Rotating group:
 O2(H2), O3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'