Synthesis and structure of a new phosphonium-1-indenylide (PHIN) ligand, 4,7-dimethyl-1-C9H4PMePh2, and of new PHIN complexes of rhodium and iridium
Purdavaie, Kourosh; Baird, Michael C.; Budzelaar, Peter H. M.; New J. Chem. 39 (2015) 9429–; doi:10.1039/C5NJ01756D

data_7055137
_publ_section_title
;
 Synthesis and structure of a new phosphonium-1-indenylide (PHIN) ligand,
 4,7-dimethyl-1-C9H4PMePh2, and of new PHIN complexes of rhodium and
 iridium
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              9429
_journal_paper_doi               10.1039/C5NJ01756D
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C24 H23 P'
_chemical_formula_sum            'C24 H23 P'
_chemical_formula_weight         342.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL-2013 template'
_audit_update_record
;
2015-07-02 deposited with the CCDC.
2015-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.4639(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.6549(2)
_cell_length_b                   11.23230(10)
_cell_length_c                   20.2304(2)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      2.36
_cell_volume                     3760.50(7)
_computing_cell_refinement
' Saint V7.68A and SADABS V2008/1 (Apex2, v2008; Bruker AXS)'
_computing_data_collection       ' APEX2 software package v2008 (Bruker AXS)'
_computing_data_reduction
' Saint V7.68A and SADABS V2008/1 (Apex2, v2008; Bruker AXS'
_computing_molecular_graphics    ' XP (SHELXTL-NT v6.14, Bruker AXS)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2012)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart Apex2 CCD (Bruker AXS)'
_diffrn_measurement_method       'CCD rotation images, \f and \w scans'
_diffrn_radiation_monochromator  'horizontal mounted graphite crystal'
_diffrn_radiation_source         'Bruker AXS K780, fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27446
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.287
_diffrn_reflns_theta_min         2.191
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Apex2, Bruker AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_transmission_factor_max   0.7455
_exptl_transmission_factor_min   0.6989
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         4206
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+2.2679P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3857
_reflns_number_total             4206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj01756d2.cif
_cod_data_source_block           mb42
_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 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7055136--7055137.cif.
;
_cod_database_code               7055137
_shelx_estimated_absorpt_t_min   0.957
_shelx_estimated_absorpt_t_max   0.971
_shelxl_version_number           2012-9
_shelx_res_checksum              69584