The Mo(CO)3 Fragment as an Organometallic Protection Group in the Synthesis of Functionalized Tripodal Phosphine Ligands
Philipp Stössel; Hermann A. Mayer; Cäcilia Maichle-Mössmer; Riad Fawzi; Manfred Steimann; Inorganic Chemistry 35 (1996) 5860–5867; doi:10.1021/ic9602512

data_4323907
_publ_section_title
;
 The Mo(CO)3 Fragment as an Organometallic Protection Group in the
 Synthesis of Functionalized Tripodal Phosphine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5860
_journal_page_last               5867
_journal_paper_doi               10.1021/ic9602512
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C63 H78 Mo N9 O9 P3'
_chemical_formula_weight         1294.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.529(3)
_cell_length_b                   30.529(3)
_cell_length_c                   13.795(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      23.4
_cell_measurement_theta_min      19.5
_cell_volume                     12857(3)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        SDP
_computing_molecular_graphics    PLATON
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      208(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       CAD4
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Cu-K\alpha
_diffrn_radiation_wavelength     1.54056
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            7119
_diffrn_reflns_theta_max         55.00
_diffrn_reflns_theta_min         5.39
_diffrn_standards_decay_%        1.2
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.878
_exptl_absorpt_correction_T_max  0.9976
_exptl_absorpt_correction_T_min  0.9421
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       bloc
_exptl_crystal_F_000             5424
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.092
_refine_ls_goodness_of_fit_obs   1.087
_refine_ls_hydrogen_treatment    calculated/determined
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         6292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_restrained_S_obs      1.087
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_obs          0.0535
_refine_ls_shift/esd_max         -4.255
_refine_ls_shift/esd_mean        0.118
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1145P)^2^+29.7931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1582
_refine_ls_wR_factor_obs         0.1532
_reflns_number_observed          6088
_reflns_number_total             6318
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9602512_1.cif
_cod_data_source_block           i82
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1145P)^2^+29.7931P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1145P)^2^+29.7931P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        12857.6
_cod_database_code               4323907