Multifunctional one-dimensional rhodium(i)-semiquinonato complex: substituent effects on crystal structures and solid-state properties.
Mitsumi, Minoru; Ohtake, Shoji; Kakuno, Yuki; Komatsu, Yuuki; Ozawa, Yoshiki; Toriumi, Koshiro; Yasuda, Nobuhiro; Azuma, Nobuaki; Miyazaki, Yuji; Inorganic chemistry 53 (2014) 11710–11720; doi:10.1021/ic5019532

data_4341347
_publ_section_title
;
 Multifunctional one-dimensional rhodium(i)-semiquinonato complex:
 substituent effects on crystal structures and solid-state properties.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11710
_journal_page_last               11720
_journal_paper_doi               10.1021/ic5019532
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C19 H24 O6 Rh'
_chemical_formula_sum            'C19 H24 O6 Rh'
_chemical_formula_weight         451.29
_chemical_name_systematic
;
 [Rh(3,6-DBSQ-4,5-PDO)(CO)2]
;
_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           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 94.592(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.0060(10)
_cell_length_b                   29.3360(10)
_cell_length_c                   21.6430(10)
_cell_measurement_reflns_used    25256
_cell_measurement_temperature    180(1)
_cell_measurement_theta_max      23.613
_cell_measurement_theta_min      2.840
_cell_volume                     3801.1(7)
_computing_cell_refinement       'SCALEPACK (Otwinoski & Minor,1997)'
_computing_data_collection       'DENZO (Otwinoski & Minor,1997)'
_computing_data_reduction        'SCALEPACK (Otwinoski & Minor,1997)'
_computing_molecular_graphics    'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-97 (A. Altomare, 1999)'
_diffrn_ambient_temperature      180(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.882
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measurement_device_type  'oscillation IP camera'
_diffrn_measurement_method       'phi-axis oscillation'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.5603
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.882
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25256
_diffrn_reflns_point_group_measured_fraction_full 0.882
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        19.644
_diffrn_reflns_theta_max         23.613
_diffrn_reflns_theta_min         2.840
_diffrn_source                   'SPring-8 8GeV synchrotron'
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_T_max  0.98471
_exptl_absorpt_correction_T_min  0.95772
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'PLATON-MULABS (A. L. Spek, 2003)'
_exptl_crystal_colour            'Dark brown'
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.395
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         9779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0599P)^2^+4.1163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8572
_reflns_number_total             9779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5019532_si_003.cif
_cod_data_source_block           '[Rh(3,6-DBSQ-4,5-PDO)(CO)2]_180K'
_cod_depositor_comments
'Adding full bibliography for 4341345--4341347.cif.'
_cod_database_code               4341347
_shelx_estimated_absorpt_t_min   0.838
_shelx_estimated_absorpt_t_max   0.986
_shelxl_version_number           2014-3
_shelx_res_checksum              99223
_shelx_hkl_checksum              65916