Thiocyanogen Insertion into P−C Bonds of Diphosphinomethanide Complexes, Leading to Rare Functionalized Diphosphine and Tetraphosphine Ligands
Ruiz, Javier; Quesada, Roberto; Vivanco, Marilín; García-Granda, Santiago; Díaz, M. Rosario; Organometallics 26 (2007) 1703–; doi:10.1021/om0611195

data_4072895
_publ_section_title
;
 Thiocyanogen Insertion into P&#x2212;C Bonds of Diphosphinomethanide
 Complexes, Leading to Rare Functionalized Diphosphine and Tetraphosphine
 Ligands
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1703
_journal_paper_doi               10.1021/om0611195
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C40 H32 Mn N5 O5 P2 S3, 2(C H2 Cl2)'
_chemical_formula_sum            'C42 H36 Cl4 Mn N5 O5 P2 S3'
_chemical_formula_weight         1045.62
_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      2.2
_audit_creation_date             2004-08-31T12:50:31-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                102.117(3)
_cell_angle_beta                 94.625(3)
_cell_angle_gamma                102.178(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1806(4)
_cell_length_b                   12.5221(6)
_cell_length_c                   17.1308(7)
_cell_measurement_reflns_used    8048
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70
_cell_measurement_theta_min      3
_cell_volume                     2272.53(17)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD control sofware (Nonius, 1997)'
_computing_data_reduction
;
 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
;
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens, 1996)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.1264
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8424
_diffrn_reflns_theta_full        69.61
_diffrn_reflns_theta_max         69.61
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    6.901
_exptl_absorpt_correction_T_max  0.355
_exptl_absorpt_correction_T_min  0.132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 multi-scan from symmetry-related measurement
        Sortav (Blessing 1995)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         8423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0462P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1394
_reflns_number_gt                7086
_reflns_number_total             8423
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0611195si20061211_114447.cif
_cod_data_source_block           14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2272.52(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4072895