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_7055136
_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         'C23 H21 P'
_chemical_formula_sum            'C23 H21 P'
_chemical_formula_weight         328.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 93.553(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3278(4)
_cell_length_b                   17.6372(8)
_cell_length_c                   12.0862(5)
_cell_measurement_reflns_used    5343
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      2.31
_cell_volume                     1771.80(14)
_computing_cell_refinement
' Saint V8.30A and SADABS V2012/1 (Apex2, v2013.10-0; Bruker AXS)'
_computing_data_collection
' APEX2 software package v2013.10-0 (Bruker AXS)'
_computing_data_reduction
' Saint V8.30A and SADABS V2012/1 (Apex2, v2013.10-0; Bruker AXS'
_computing_molecular_graphics    ' XP (SHELXTL-NT v6.14, Bruker AXS)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    ' 'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15480
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.208
_diffrn_reflns_theta_min         2.045
_diffrn_source                   'Bruker AXS K780, fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_T_max  0.7421
_exptl_absorpt_correction_T_min  0.7023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2012/1 (Apex2, Bruker AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.158
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+0.5900P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2994
_reflns_number_total             3945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj01756d2.cif
_cod_data_source_block           mbkp_205_0m
_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               7055136
_shelx_estimated_absorpt_t_min   0.968
_shelx_estimated_absorpt_t_max   0.976
_shelxl_version_number           2012-9
_shelx_res_checksum              29390