Crystal polymorphism and crystalline-state photochromism of a rhodium dithionite complex with n-methoxypropyl moieties
Kajiwara, Yuu; Nakai, Hidetaka; CrystEngComm  (2022) –; doi:10.1039/D1CE01613J

data_7244159
_publ_section_title
;
 Crystal polymorphism and crystalline-state photochromism of a rhodium
 dithionite complex with n-methoxypropyl moieties
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D1CE01613J
_journal_year                    2022
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C28 H46 O6 Rh2 S2'
_chemical_formula_sum            'C28 H46 O6 Rh2 S2'
_chemical_formula_weight         748.60
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-12-04 deposited with the CCDC.	2022-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 102.509(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.0170(5)
_cell_length_b                   26.3115(11)
_cell_length_c                   10.1716(4)
_cell_measurement_reflns_used    7661
_cell_measurement_temperature    296
_cell_measurement_theta_max      30.41
_cell_measurement_theta_min      3.11
_cell_volume                     3139.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2.2'
_computing_publication_material  'CrystalStructure 4.2.2 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17546
_diffrn_reflns_point_group_measured_fraction_full 0.885
_diffrn_reflns_point_group_measured_fraction_max 0.749
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.165
_diffrn_reflns_theta_min         3.060
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.219
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.99
_refine_diff_density_min         -0.35
_refine_ls_abs_structure_details
;
 Flack x determined using 2556 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     371
_refine_ls_number_reflns         7597
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.8455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0792
_reflns_Friedel_coverage         0.671
_reflns_Friedel_fraction_full    0.771
_reflns_Friedel_fraction_max     0.602
_reflns_number_gt                6869
_reflns_number_total             7597
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d1ce01613j2.cif
_cod_data_source_block           sample4
_cod_database_code               7244159
_shelx_res_checksum              67641