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_4517452
_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 Cr O7, H2 O'
_chemical_formula_sum            'C4 H5 Cr O8'
_chemical_formula_weight         233.08
_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                106.303(9)
_cell_angle_beta                 95.252(10)
_cell_angle_gamma                113.775(10)
_cell_formula_units_Z            2
_cell_length_a                   7.489(4)
_cell_length_b                   7.545(4)
_cell_length_c                   8.142(4)
_cell_measurement_reflns_used    1941
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.084
_cell_measurement_theta_min      2.679
_cell_volume                     393.0(4)
_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  'XH (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 8.34
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.933
_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  0.0592
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3648
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         2.68
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           32.0
_diffrn_source_power             1.6
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.470
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.079947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SAD V2.05 (BRUKER, 2001) was used for absorption correction. R(int) was 0.0497 before and 0.0151 after correction. The Ratio of minimum to maximum transmission is 0.0799. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             234
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.6740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1316
_reflns_number_gt                1706
_reflns_number_total             1828
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ao0c00083_si_002.cif
_cod_data_source_block           wgv4s
_cod_database_code               4517452
_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'