Mononuclear anionic AO2X3 compounds with non-VSEPR structure.
García-Monforte, M Angeles; Baya, Miguel; Betoré, M Pilar; Martín, Antonio; Menjón, Babil; Dalton transactions (Cambridge, England : 2003) 43 (2014) 7615–7621; doi:10.1039/c4dt00525b

data_7030360
_publ_section_title
;
 Mononuclear anionic AO2X3 compounds with non-VSEPR structure.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7615
_journal_page_last               7621
_journal_paper_doi               10.1039/c4dt00525b
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C34.25 H36.5 Cl0.5 F15 Mo N O2'
_chemical_formula_weight         892.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.063(3)
_cell_angle_beta                 84.902(3)
_cell_angle_gamma                83.183(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1922(3)
_cell_length_b                   12.9530(4)
_cell_length_c                   13.1007(5)
_cell_measurement_reflns_used    5548
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8108
_cell_measurement_theta_min      4.1504
_cell_volume                     1847.27(11)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -52.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615   77.0000 -150.0000 102

  2 omega   12.00   50.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615   77.0000 -120.0000 38

  3 omega  -49.00   42.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615   77.0000  120.0000 91

  4 omega  -11.00   35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9928   77.0000   90.0000 46

  5 omega   64.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9928   77.0000    0.0000 25

  6 omega  -11.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9928   77.0000  -30.0000 99

  7 omega  -93.00   12.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  -37.0000  150.0000 105

  8 omega  -91.00    4.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  -57.0000   90.0000 95

  9 omega   -2.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9928   57.0000  -60.0000 95

 10 omega   34.00  102.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9928  179.0000 -180.0000 68

 11 omega   34.00  102.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9928  179.0000   90.0000 68

 12 omega  -25.00   67.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9928  -99.0000  -30.0000 92

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'w scans'
_diffrn_orient_matrix_UB_11      0.0470706696
_diffrn_orient_matrix_UB_12      0.0211592287
_diffrn_orient_matrix_UB_13      -0.0346228705
_diffrn_orient_matrix_UB_21      0.0417529925
_diffrn_orient_matrix_UB_22      -0.0413209829
_diffrn_orient_matrix_UB_23      0.0233905485
_diffrn_orient_matrix_UB_31      -0.0113517875
_diffrn_orient_matrix_UB_32      -0.0313788581
_diffrn_orient_matrix_UB_33      -0.0361444239
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1098
_diffrn_reflns_av_sigmaI/netI    0.1750
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27884
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         4.16
_exptl_absorpt_coefficient_mu    0.499
_exptl_absorpt_correction_T_max  0.9803
_exptl_absorpt_correction_T_min  0.8687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             901
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         6848
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0812
_reflns_number_gt                3474
_reflns_number_total             6848
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00525b2.cif
_cod_data_source_block           amt684
_cod_original_cell_volume        1847.26(11)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C34.25 H36.50 Cl0.50 F15 Mo N O2'
_cod_database_code               7030360