Versatile heteroleptic bis-terdentate Cr(iii) chromophores displaying room temperature millisecond excited state lifetimes.
Jiménez, Juan-Ramón; Doistau, Benjamin; Besnard, Céline; Piguet, Claude; Chemical communications (Cambridge, England) 54 (2018) 13228–13231; doi:10.1039/c8cc07671e

data_7122544
_publ_section_title
;
 Versatile heteroleptic bis-terdentate Cr(iii) chromophores displaying
 room temperature millisecond excited state lifetimes.
;
_journal_issue                   94
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              13228
_journal_page_last               13231
_journal_paper_doi               10.1039/c8cc07671e
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C32 H28 Cr N8, 3(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C36 H34 Cr F18 N10 P3'
_chemical_formula_weight         1093.64
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-20 deposited with the CCDC.
2018-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0625(3)
_cell_length_b                   16.1756(3)
_cell_length_c                   13.5227(2)
_cell_measurement_reflns_used    9306
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      77.7420
_cell_measurement_theta_min      3.4790
_cell_volume                     4388.43(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_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    -63.00  21.00   0.50    0.42    --  -49.30  71.00   4.00  168
  2  \w   -122.00 -74.00   0.50    1.67    --  -84.25-132.00 173.00   96
  3  \w   -111.00 -68.00   0.50    1.67    --  -84.25 -71.00-126.00   86
  4  \w    -82.00 -23.00   0.50    1.67    --  -84.25  49.00-169.00  118
  5  \w     97.00 168.00   0.50    1.67    --  105.75  49.00-169.00  142
  6  \w    -80.00 -43.00   0.50    0.42    --  -49.30   0.00-180.00   74
  7  \w   -110.00 -70.00   0.50    0.42    --  -49.30-125.00   0.00   80
  8  \w     34.00 109.00   0.50    1.67    --  105.75 -99.00   0.00  150
  9  \w     34.00  71.00   0.50    1.67    --  105.75 -37.00  90.00   74
 10  \w     34.00  96.00   0.50    1.67    --  105.75 -57.00 150.00  124
 11  \w     57.00 112.00   0.50    1.67    --  105.75   0.00-150.00  110
 12  \w     63.00 108.00   0.50    1.67    --  105.75   0.00  60.00   90
 13  \w     34.00 109.00   0.50    1.67    --  105.75-125.00 -30.00  150
 14  \w     38.00  71.00   0.50    1.67    --  105.75 -37.00 -90.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0675975000
_diffrn_orient_matrix_UB_12      -0.0368418000
_diffrn_orient_matrix_UB_13      0.0314159000
_diffrn_orient_matrix_UB_21      0.0364701000
_diffrn_orient_matrix_UB_22      0.0661932000
_diffrn_orient_matrix_UB_23      -0.0617096000
_diffrn_orient_matrix_UB_31      0.0013622000
_diffrn_orient_matrix_UB_32      0.0577008000
_diffrn_orient_matrix_UB_33      0.0904233000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24416
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.171
_diffrn_reflns_theta_min         3.510
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.274
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_description       block
_exptl_crystal_F_000             2204
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.103
_refine_diff_density_max         1.515
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.003(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         7452
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0515P)^2^+8.1337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1204
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                7210
_reflns_number_total             7452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07671e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7122544--7122546.cif.'
_cod_original_cell_volume        4388.40(12)
_cod_database_code               7122544
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C36 H35 Cr1 F18 N10 P3'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.997(8)
 0.003(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26),
 C29(H29), C30(H30), C31(H31), C32(H32), C17(H17), C16(H16), C15(H15), C14(H14),
  C10(H10), C9(H9), C8(H8), C4(H4), C3(H3), C2(H2), C1(H1)
3.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C6(H6A,H6B,H6C), C35(H35A,H35B,H35C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              7169
_shelx_hkl_checksum              42088
_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 1.587
_oxdiff_exptl_absorpt_empirical_full_min 0.816