<i>mer</i>-Hydridotris(trimethylphosphane-κ<i>P</i>)(<small>D</small>-valinato-κ^2^<i>N</i>,<i>O</i>)iridium hexafluoridophosphate dichloromethane 0.675-solvate
Merola, Joseph S.; Slebodnick, Carla; Berg, Michael; Ritchie, Melissa K.; Acta Crystallographica Section E 70 (2014) m82–; doi:10.1107/S1600536814002165

data_2239399
_publ_section_title
;
 <i>mer</i>-Hydridotris(trimethylphosphane-\k<i>P</i>)(<small>D</small>-valinato-\k^2^<i>N</i>,<i>O</i>)iridium
 hexafluoridophosphate dichloromethane 0.675-solvate
;
_journal_coeditor_code           PK2516
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m82
_journal_paper_doi               10.1107/S1600536814002165
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac
'[Ir (C5 H10 N O2) H (C3 H9 P)3] P F6, 0.675C H2 Cl2'
_chemical_formula_moiety         'C14 H38 Ir N O2 P3, F6 P, 0.675(C1 H2 Cl2)'
_chemical_formula_sum            'C14.68 H39.35 Cl1.35 F6 Ir N O2 P4'
_chemical_formula_weight         739.86
_chemical_name_systematic
;<i>mer</i>-Hydridotris(trimethylphosphane-\k<i>P</i>)(<i>D</i>-valinato-\k^2^<i>N</i>,<i>O</i>)iridium hexafluoridophosphate dichloromethane
0.675-solvate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           76
_space_group_name_Hall           'P 4w'
_space_group_name_H-M_alt        'P 41'
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.04454(17)
_cell_length_b                   14.04454(17)
_cell_length_c                   14.2657(3)
_cell_measurement_reflns_used    12856
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4173
_cell_measurement_theta_min      3.5096
_cell_volume                     2813.90(8)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_molecular_graphics    'OLEX2 (Dolomanov <i>et al.</i>, 2009)'
_computing_publication_material  'OLEX2 (Dolomanov <i>et al.</i>, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 16.0122
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur2 (Eos, Gemini ultra)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39354
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         31.488
_diffrn_reflns_theta_min         3.517
_exptl_absorpt_coefficient_mu    5.152
_exptl_absorpt_correction_T_max  0.774
_exptl_absorpt_correction_T_min  0.449
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2010)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_description       needle
_exptl_crystal_F_000             1457
_exptl_crystal_size_max          0.1654
_exptl_crystal_size_mid          0.0511
_exptl_crystal_size_min          0.0506
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.607
_refine_ls_abs_structure_details
;
Flack parameter determined using 3004 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   -0.021(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.805
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         9371
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.806
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0307
_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^)+(0.0129P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0446
_refine_ls_wR_factor_ref         0.0461
_reflns_number_gt                7266
_reflns_number_total             9371
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2516sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2813.89(9)
_cod_database_code               2239399
_cod_database_fobs_code          2239399
_shelxl_version_number           2.013