Crystal structures offac-trichloridotris(trimethylphosphane-κP)rhodium(III) monohydrate andfac-trichloridotris(trimethylphosphane-κP)rhodium(III) methanol hemisolvate: rhodium structures that are isotypic with their iridium analogs
Merola, Joseph S.; Franks, Marion A.; Acta Crystallographica Section E Crystallographic Communications 71 (2015) 226–; doi:10.1107/S2056989015001516

data_2019822
_publ_section_title
;
 Crystal structures
 offac-trichloridotris(trimethylphosphane-\kP)rhodium(III) monohydrate
 andfac-trichloridotris(trimethylphosphane-\kP)rhodium(III) methanol
 hemisolvate: rhodium structures that are isotypic with their iridium
 analogs
;
_journal_issue                   2
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              226
_journal_paper_doi               10.1107/S2056989015001516
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Rh Cl3 (C3 H9 P)3], 0.5C H4 O'
_chemical_formula_moiety         'C9 H27 Cl3 P3 Rh, 0.5(C H4 O)'
_chemical_formula_sum            'C9.5 H29 Cl3 O0.5 P3 Rh'
_chemical_formula_weight         453.50
_chemical_name_systematic
;
<i>fac</i>-Trichloridotris(trimethylphosphane-\k<i>P</i>)rhodium
methanol hemisolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled Nov 28 2014 11:48:57 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 115.084(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.0993(16)
_cell_length_b                   15.5910(9)
_cell_length_c                   16.4152(14)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    298
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     3731.7(7)
_computing_cell_refinement
;
XSCANS (Siemens, 1996)
;
_computing_data_collection
;
XSCANS (Siemens, 1996)
;
_computing_data_reduction
;
XSCANS (Siemens, 1996)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS87 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       'sea;ed X-ray tube'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5957
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0.0(2)
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_T_max  0.9153
_exptl_absorpt_correction_T_min  0.8070
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
(North <i>et al.</i>,  1968)
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.031
_refine_diff_density_min         -0.408
_refine_ls_extinction_coef       0.00519(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         4858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+4.1793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                4171
_reflns_number_total             4858
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            pk2543sup1.cif
_cod_data_source_block           RhP3Cl3MeOH
_cod_original_cell_volume        3731.7(5)
_cod_original_formula_sum        'C9.5 H29 Cl3 O0.5 P3 Rh1'
_cod_database_code               2019822
_cod_database_fobs_code          2019822