Single Crystal X-ray Diffraction Studies of Two Polymorphic Modifications of the Dicarbonyl-<i>o</i>-Semiquinonato Rhodium Complex at Different Temperatures. Destruction Stimulated by Cooling Versus Stability.
Rumyantcev, Roman V.; Fukin, Georgy K.; Romanenko, Galina V.; Teplova, Irina A.; Bubnov, Michael P.; Cherkasov, Vladimir K.; ACS omega 5 (2020) 32792–32799; doi:10.1021/acsomega.0c05344

data_4518302
_publ_section_title
;
 Single Crystal X-ray Diffraction Studies of Two Polymorphic Modifications
 of the Dicarbonyl-<i>o</i>-Semiquinonato Rhodium Complex at Different
 Temperatures. Destruction Stimulated by Cooling Versus Stability.
;
_journal_issue                   50
_journal_name_full               'ACS omega'
_journal_page_first              32792
_journal_page_last               32799
_journal_paper_doi               10.1021/acsomega.0c05344
_journal_volume                  5
_journal_year                    2020
_chemical_formula_sum            'C16 H20 O4 Rh'
_chemical_formula_weight         379.23
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.0030(13)
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_cell_length_a                   6.6304(2)
_cell_length_b                   21.0748(7)
_cell_length_c                   23.9202(7)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.61
_cell_measurement_theta_min      2.73
_cell_volume                     3342.47(18)
_computing_cell_refinement       SAINT
_computing_data_collection       APEX3
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXL-2014/7
_computing_structure_solution    SHELXT-2014/5
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest (CMOS)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            48630
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_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.554
_diffrn_source                   'microfocus tube'
_exptl_absorpt_coefficient_mu    1.033
_exptl_absorpt_correction_T_max  0.8496
_exptl_absorpt_correction_T_min  0.7348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       stick
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         8281
_refine_ls_number_restraints     354
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1429
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+2.9123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3772
_reflns_number_total             8281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c05344_si_003.cif
_cod_data_source_block           2_298_1
_cod_depositor_comments
'Adding full bibliography for 4518296--4518313.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4518302
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.659
_shelx_estimated_absorpt_t_max   0.941
_shelx_res_checksum              35933
_shelx_hkl_checksum              12327