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_2019821
_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_coeditor_code           PK2543
_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], H2 O'
_chemical_formula_moiety         'C9 H27 Cl3 P3 Rh, H2 O'
_chemical_formula_sum            'C9 H29 Cl3 O P3 Rh'
_chemical_formula_weight         455.49
_chemical_name_systematic
;
<i>fac</i>-Trichloridotris(trimethylphosphane-\k<i>P</i>)rhodium
monohydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
;
_cell_angle_alpha                90
_cell_angle_beta                 120.820(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8650(12)
_cell_length_b                   9.0396(3)
_cell_length_c                   14.8223(18)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    298
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     1825.5(3)
_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
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       Wyckoff
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2034
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.704
_diffrn_standards_decay_%        0.0(2)
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.623
_exptl_absorpt_correction_T_max  0.97358
_exptl_absorpt_correction_T_min  0.76208
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
(North <i>et al.</i>,  1968)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       prism
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.597
_refine_ls_abs_structure_details
;
Classical Flack (1983) method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.06(3)
_refine_ls_extinction_coef       0.0052(3)
_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   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         1784
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0359P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0585
_reflns_number_gt                1763
_reflns_number_total             1784
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2543sup1.cif
_cod_data_source_block           RhP3Cl3water
_cod_database_code               2019821
_shelx_hkl_checksum              5450
_shelx_res_checksum              34702