A convenient method for selective substitutions at the backbone of a co-ordinated imidazolylphosphine P‒N ligand. Single crystal X-ray analyses of [Mo(CO)4(MeImCH2PPh2)] and its ethyl substituted derivative [Mo(CO)4(MeImCHEtPPh2)] †
Jalil, M. Abdul; Fujinami, Shuhei; Nishikawa, Hiroaki; Journal of the Chemical Society, Dalton Transactions  (1999) 3499–; doi:10.1039/a905186d

data_7027658
_publ_section_title
;
 A convenient method for selective substitutions at the backbone of a
 co-ordinated imidazolylphosphine P--N ligand. Single crystal X-ray
 analyses of [Mo(CO)4(MeImCH2PPh2)] and its ethyl substituted derivative
 [Mo(CO)4(MeImCHEtPPh2)]&#x200A;&#x2020;
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3499
_journal_paper_doi               10.1039/a905186d
_journal_year                    1999
_chemical_formula_moiety         'C21 H17 N2 Mo O4 P '
_chemical_formula_sum            'C21 H17 Mo N2 O4 P'
_chemical_formula_weight         488.29
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             'Thu Jun 24 15:41:29 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 108.266(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.554(1)
_cell_length_b                   7.617(1)
_cell_length_c                   17.100(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.9
_cell_volume                     2171.2(3)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.02937
_diffrn_orient_matrix_UB_12      0.01535
_diffrn_orient_matrix_UB_13      0.04108
_diffrn_orient_matrix_UB_21      -0.05223
_diffrn_orient_matrix_UB_22      -0.00172
_diffrn_orient_matrix_UB_23      -0.04556
_diffrn_orient_matrix_UB_31      -0.00277
_diffrn_orient_matrix_UB_32      -0.13038
_diffrn_orient_matrix_UB_33      0.00544
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.006
_diffrn_reflns_av_sigmaI/netI    0.021
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5494
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         5.01
_diffrn_standards_decay_%        -0.36
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             984.00
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.46
_refine_ls_extinction_coef       0.005(2)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_obs   1.313
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4218
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0263
_refine_ls_shift/esd_max         0.0040
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00109|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0504
_reflns_number_observed          4218
_reflns_number_total             5327
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            905186dsup1.cif
_cod_data_source_block           '[Mo(CO)4(MeImCH2PPh2)]'
_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 'w = 1/[\s^2^(Fo) +
0.00109|Fo|^2^]' 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) + 0.00109|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2171.2(4)
_cod_original_sg_symbol_H-M      'P 21/c       '
_cod_original_formula_sum        'C21 H17 N2 Mo O4 P '
_cod_database_code               7027658