DCM self-trapping by the host deformation in flexible host–guest molecules
Miao, Le-Ping; Qi, Qi; Han, Xiang-Bin; Zhang, Wen; CrystEngComm 23 (2021) 4136–4142; doi:10.1039/D1CE00301A

data_7242700
_publ_section_title
;
 DCM self-trapping by the host deformation in flexible host--guest
 molecules
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              4136
_journal_page_last               4142
_journal_paper_doi               10.1039/D1CE00301A
_journal_volume                  23
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H28 Ir N3 O2, 1.5(C H Cl3)'
_chemical_formula_sum            'C37.5 H29.5 Cl4.5 Ir N3 O2'
_chemical_formula_weight         905.86
_chemical_properties_physical    Light-sensitive,Photo-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc26wt64
_audit_creation_date             2018-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-26 deposited with the CCDC.	2021-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.568(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6933(6)
_cell_length_b                   19.4475(9)
_cell_length_c                   15.7924(7)
_cell_measurement_reflns_used    8156
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.0710
_cell_measurement_theta_min      4.0240
_cell_volume                     3475.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -3.00  89.00   1.00   32.50    --   12.86  38.00 150.00   92
  2  \w    -63.00  39.00   1.00   32.50    --   12.86 -38.00-180.00  102
  3  \w    -18.00  81.00   1.00   32.50    --   12.86  77.00   0.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0263095000
_diffrn_orient_matrix_UB_12      0.0239752000
_diffrn_orient_matrix_UB_13      -0.0232031000
_diffrn_orient_matrix_UB_21      0.0561603000
_diffrn_orient_matrix_UB_22      -0.0069264000
_diffrn_orient_matrix_UB_23      0.0285033000
_diffrn_orient_matrix_UB_31      0.0091050000
_diffrn_orient_matrix_UB_32      -0.0266168000
_diffrn_orient_matrix_UB_33      -0.0282990000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.1014
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25818
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.48
_diffrn_reflns_theta_min         3.39
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.226
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1780
_refine_diff_density_max         1.806
_refine_diff_density_min         -1.833
_refine_diff_density_rms         0.172
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.025(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         15859
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0639P)^2^+6.2424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1396
_reflns_number_gt                12308
_reflns_number_total             15859
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1ce00301a2.cif
_cod_data_source_block           exp_216
_cod_depositor_comments
;
Adding full bibliography for 7242699--7242712.cif.

2024-11-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C75 H59 Cl9 Ir2 N6 O4'
_cod_original_formula_weight         1811.73
_cod_original_formula_moiety         '2(C36 H28 Ir N3 O2), 3(C H Cl3)'
_cod_original_formula_units_Z            2
_cod_database_code               7242700
_chemical_oxdiff_formula         CHONIr
_chemical_oxdiff_usercomment     180522PHL
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Cl7)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C17) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl1) \\sim Ueq, Uanis(Cl7) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C73(H73), C75(H75), C74(H74)
3.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C35(H35A,H35B), C34(H34A,H34B), C33(H33A,H33B), C72(H72A,
 H72B), C71(H71A,H71B), C70(H70A,H70B), C69(H69A,H69B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C14(H14), C13(H13), C12(H12),
 C11(H11), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C29(H29),
  C28(H28), C27(H27), C26(H26), C53(H53), C54(H54), C55(H55), C56(H56),
 C59(H59), C60(H60), C65(H65), C64(H64), C63(H63), C62(H62), C38(H38), C39(H39),
  C40(H40), C41(H41), C44(H44), C45(H45), C50(H50), C49(H49), C48(H48), C47(H47)
;
_olex2_date_sample_data_collection 2018-05-22
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.242
_oxdiff_exptl_absorpt_empirical_full_min 0.836