Design and photophysical studies of iridium(iii)-cobalt(iii) dyads and their application for dihydrogen photo-evolution.
Lentz, Cédric; Schott, Olivier; Auvray, Thomas; Hanan, Garry S.; Elias, Benjamin; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15567–15576; doi:10.1039/c9dt01989h

data_7700647
_publ_section_title
;
 Design and photophysical studies of iridium(iii)-cobalt(iii) dyads and
 their application for dihydrogen photo-evolution.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15567
_journal_page_last               15576
_journal_paper_doi               10.1039/c9dt01989h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C37 H27 Ir N5, F6 P'
_chemical_formula_sum            'C37 H27 F6 Ir N5 P'
_chemical_formula_weight         878.80
_chemical_name_systematic
'Ir(phenylisoquinoline)2(2,2,4,4 terpyridine)PF6'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-26 deposited with the CCDC.    2019-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.834(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.5798(19)
_cell_length_b                   24.646(2)
_cell_length_c                   14.4517(13)
_cell_measurement_reflns_used    9482
_cell_measurement_temperature    100
_cell_measurement_theta_max      60.52
_cell_measurement_theta_min      2.52
_cell_volume                     6937.6(11)
_computing_cell_refinement
;
SAINT () ; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_collection
;
APEX 2 () Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction
;
SAINT () ; Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.
;
_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    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15701
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.798
_diffrn_reflns_theta_min         2.515
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.604
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 126312 reflections, Rint = 0.0844
 (105284 with I > 3sig(I), Rint = 0.0834)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       needle
_exptl_crystal_F_000             3440
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Slow diffusion of disopropylether into acetonitrile'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.323
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         7954
_refine_ls_number_restraints     353
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0710
_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^)+(0.0804P)^2^+139.9823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.1835
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6736
_reflns_number_total             7954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01989h2.cif
_cod_data_source_block           schot4_sq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_colour_primary' value 'Yellow' changed to 'yellow'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7700646--7700648.cif.
;
_cod_original_cell_volume        6937.7(11)
_cod_database_code               7700647
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F18-F17 = F16-F15 = F14-F13
 2.27 with sigma of 0.02
 F6-F5 = F4-F3 = F2-F1
 2.27 with sigma of 0.02
 F12-F11 = F10-F9 = F8-F7
 2.27 with sigma of 0.02
 P3-F18
 1.6 with sigma of 0.02
 P3-F17
 1.6 with sigma of 0.02
 P3-F16
 1.6 with sigma of 0.02
 P3-F15
 1.6 with sigma of 0.02
 P3-F14
 1.6 with sigma of 0.02
 P3-F13
 1.6 with sigma of 0.02
 P2-F12
 1.6 with sigma of 0.02
 P2-F11
 1.6 with sigma of 0.02
 P2-F10
 1.6 with sigma of 0.02
 P2-F9
 1.6 with sigma of 0.02
 P2-F8
 1.6 with sigma of 0.02
 P2-F7
 1.6 with sigma of 0.02
 P1-F6
 1.6 with sigma of 0.02
 P1-F5
 1.6 with sigma of 0.02
 P1-F4
 1.6 with sigma of 0.02
 P1-F3
 1.6 with sigma of 0.02
 P1-F2
 1.6 with sigma of 0.02
 P1-F1
 1.6 with sigma of 0.02
 P1-F2
 1.6 with sigma of 0.04
 P1-F1
 1.6 with sigma of 0.04
 P1-F3
 1.6 with sigma of 0.04
 P1-F5
 1.6 with sigma of 0.04
 P1-F4
 1.6 with sigma of 0.04
 P1-F6
 1.6 with sigma of 0.04
 F1-F3
 2.27 with sigma of 0.04
 F3-F2
 2.27 with sigma of 0.04
 F1-F2
 2.27 with sigma of 0.04
 F1-F6
 2.27 with sigma of 0.04
 F2-F6
 2.27 with sigma of 0.04
 F5-F6
 2.27 with sigma of 0.04
 F4-F6
 2.27 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.002 and sigma
for terminal atoms of 0.002
Uiso(F1) = Uiso(F7)
Uiso(F2) = Uiso(F8)
Uiso(F3) = Uiso(F9)
Uiso(F1) = Uiso(F13)
Uiso(F2) = Uiso(F13)
Uiso(F3) = Uiso(F13)
Uiso(P1) = Uiso(P3)
4. Others
 Sof(P2)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=0.5*(1-FVAR(2))
 Sof(P1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=0.5*FVAR(2)
 Fixed Sof: P3(0.5) F13(0.5) F14(0.5) F15(0.5) F16(0.5) F17(0.5) F18(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C19(H19), C21(H21),
 C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32),
  C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C110(H110), C113(H113),
 C114(H114), C115(H115), C116(H116), C210(H210), C310(H310)
;
_shelx_res_checksum              59771
_shelx_fab_checksum              26945
_olex2_submission_special_instructions 'No special instructions were received'