Template Synthesis and Reactions of Tricarbonylmolybdenum Phosphadithiamacrocycle Complexes
Philip J. Blower; John C. Jeffery; John R. Miller; Spencer N. Salek; Dirk Schmaljohann; Raymond J. Smith; Michael J. Went; Inorganic Chemistry 36 (1997) 1578–1582; doi:10.1021/ic961143i

data_4323379
_publ_contact_author
;
    Dr. J.R. Miller
    Dept. of Biological and Chemical Sciences
    Central Campus
    University of Essex
    Wivenhoe Park
    Colchester  CO4 3SQ
    UK
;
_publ_contact_author_email       john@essex.ac.uk
_publ_contact_author_phone       '01206 87 2117'
_publ_section_title
;
 Template Synthesis and Reactions of Tricarbonylmolybdenum
 Phosphadithiamacrocycle Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1578
_journal_page_last               1582
_journal_paper_doi               10.1021/ic961143i
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C12 H17 P S3'
_chemical_formula_weight         288.44
_chemical_name_systematic
' 1-phenyl,1-sulfido(1-phospha-4,7-dithiacyclononane)'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_type_scat_source           International_Tables_for_Xray_Crystallography
_cell_angle_alpha                90.00
_cell_angle_beta                 101.62(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.650(4)
_cell_length_b                   7.313(2)
_cell_length_c                   14.687(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    291
_cell_measurement_theta_max      25
_cell_measurement_theta_min      22
_cell_volume                     699.6(6)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        PROCESS_MolEN_(Fair,_1990)
_computing_molecular_graphics    ORTEP_(Johnson,_1976)
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  LSFM_MolEN_(Fair,_1990)
_computing_structure_solution    'Direct_methods_SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291
_diffrn_measurement_device       Enraf_Nonius_CAD4
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            1455
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.78
_diffrn_standards_decay_%        1.20
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  0.9993
_exptl_absorpt_correction_T_min  0.7307
_exptl_absorpt_correction_type   '9 \Y-scans (Fair, 1990)'
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.37
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.81
_refine_diff_density_min         -0.66
_refine_ls_abs_structure_details
;
?
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   3.857
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         1251
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.077
_refine_ls_R_factor_obs          0.070
_refine_ls_shift/esd_max         0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/ (\s^2^(Fo^2^) + 0.0016 Fo^4^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.096
_reflns_number_observed          1251
_reflns_number_total             1340
_reflns_observed_criterion       >1.5\s(I)
_cod_data_source_file            ic961143i_4.cif
_cod_data_source_block           mjw1_ars3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/ (\s^2^(Fo^2^) + 0.0016
Fo^4^)' was changed to 'calc'. New tag '_refine_ls_weighting_details'
was created. The value of the new tag was set to 'w = 4Fo^2^/
(\s^2^(Fo^2^) + 0.0016 Fo^4^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        700(1)
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C12 H17 P1 S3'
_cod_database_code               4323379