Vapor switching of the luminescence mechanism in a Re(V) complex.
Sasaki, Kenta; Yamate, Hitomi; Yoshino, Haruka; Miura, Hiroki; Shimoda, Yuushi; Miyata, Kiyoshi; Onda, Ken; Ohtani, Ryo; Ohba, Masaaki; Chemical communications (Cambridge, England) 56 (2020) 12961–12964; doi:10.1039/d0cc05462c

data_7127297
_publ_section_title
;
 Vapor switching of the luminescence mechanism in a Re(V) complex.
;
_journal_issue                   85
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12961
_journal_page_last               12964
_journal_paper_doi               10.1039/d0cc05462c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C5 H3 N5 O Re, 2(C24 H20 P), 2(C O), 2(O)'
_chemical_formula_sum            'C55 H43 N5 O5 P2 Re'
_chemical_formula_weight         1102.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc25g9qp
_audit_creation_date             2020-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-15 deposited with the CCDC.	2020-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                71.036(2)
_cell_angle_beta                 89.469(2)
_cell_angle_gamma                61.390(2)
_cell_formula_units_Z            2
_cell_length_a                   13.437(2)
_cell_length_b                   13.848(2)
_cell_length_c                   16.639(3)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.37
_cell_volume                     2530.3(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24962
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.378
_diffrn_reflns_theta_min         1.315
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.517
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0667 before and 0.0393 after correction.
The Ratio of minimum to maximum transmission is 0.7977.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             1106
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.065
_refine_diff_density_max         2.376
_refine_diff_density_min         -1.757
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         10162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0304P)^2^+9.0344P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8908
_reflns_number_total             10162
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05462c2.cif
_cod_data_source_block           190831_re_4cypy_meoh3_0m_a
_cod_depositor_comments
'Adding full bibliography for 7127296--7127298.cif.'
_cod_original_cell_volume        2530.4(7)
_cod_database_code               7127297
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.657
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O2A(0.5) O2B(0.5) O3A(0.5) O3B(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27),
  C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35),
 C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C45(H45),
  C46(H46), C47(H47), C48(H48), C49(H49), C51(H51), C52(H52), C53(H53),
 C54(H54), C55(H55)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_shelx_res_checksum              16309
_shelx_hkl_checksum              38154
_olex2_submission_original_sample_id 2
_olex2_submission_special_instructions 'No special instructions were received'