Phosphinoarylthiolato molybdenum and iron complexes [M{(SC6H4-2-PPh2)-k2S,P}2(CO)2] (M = Mo, Fe): Analogous composition - Different structure
Ana-Maria Valean; Santiago Gomez-Ruiz; Alexandru Lupan; Radu Silaghi-Dumitrescu; Luminita Silaghi-Dumitrescu; Evamarie Hey-Hawkins; Inorganica Chimica Acta 394 (2013) 289–294; doi:10.1016/j.ica.2012.05.041

data_1512753
_publ_section_title
;
 Phosphinoarylthiolato molybdenum and iron complexes
 [M{(SC6H4-2-PPh2)-k2S,P}2(CO)2] (M = Mo, Fe): Analogous composition -
 Different structure
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              289
_journal_page_last               294
_journal_paper_doi               10.1016/j.ica.2012.05.041
_journal_volume                  394
_journal_year                    2013
_chemical_formula_sum            'C41.5 H32 Mo O2 P2 S2'
_chemical_formula_weight         784.67
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2007-01-18T10:13:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                98.310(5)
_cell_angle_beta                 95.226(5)
_cell_angle_gamma                95.226(5)
_cell_formula_units_Z            2
_cell_length_a                   11.062(5)
_cell_length_b                   13.024(5)
_cell_length_c                   13.025(5)
_cell_measurement_reflns_used    9678
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      32.2914
_cell_measurement_theta_min      2.561
_cell_volume                     1838.7(13)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
        (compiled Oct 18 2006,16:28:17)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector_area_resol_mean 16.356
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ccd xcalibur s'
_diffrn_measurement_method       '\w scans and \f scans'
_diffrn_orient_matrix_UB_11      0.0275321355
_diffrn_orient_matrix_UB_12      0.0264223541
_diffrn_orient_matrix_UB_13      0.0158526357
_diffrn_orient_matrix_UB_21      -0.0281674809
_diffrn_orient_matrix_UB_22      0.017436071
_diffrn_orient_matrix_UB_23      0.0300450012
_diffrn_orient_matrix_UB_31      0.0143378668
_diffrn_orient_matrix_UB_32      -0.0168894329
_diffrn_orient_matrix_UB_33      0.0548960261
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_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            36961
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                4744
_reflns_number_total             6976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-394-289-294-1.cif
_cod_data_source_block           x0129fin
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C41.50 H32 Mo O2 P2 S2'
_cod_database_code               1512753