Panchromatic dirhodium photocatalysts for dihydrogen generation with red light
Huang, Jie; Gallucci, Judith C.; Turro, Claudia; Chemical Science 11 (2020) 9775–9783; doi:10.1039/D0SC03114C

data_1559176
_publ_section_title
;
 Panchromatic dirhodium photocatalysts for dihydrogen generation with red
 light
;
_journal_issue                   36
_journal_name_full               'Chemical Science'
_journal_page_first              9775
_journal_page_last               9783
_journal_paper_doi               10.1039/D0SC03114C
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C66 H52 N10 Rh2, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C68 H55 B2 F8 N11 Rh2'
_chemical_formula_weight         1405.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-12-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-28 deposited with the CCDC.	2020-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.4260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2611(7)
_cell_length_b                   37.3119(18)
_cell_length_c                   14.5988(7)
_cell_measurement_reflns_used    9593
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      26.375
_cell_measurement_theta_min      2.860
_cell_volume                     7015.7(6)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_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_temperature      150.0
_diffrn_detector                 'Bruker Photon II area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Curved-Graphite, Bruker TRIUMPH'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            135826
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.403
_diffrn_reflns_theta_min         2.914
_diffrn_source                   'sealed tube'
_diffrn_source_type              fine-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0634 before and 0.0522 after correction. The Ratio of minimum to maximum transmission is 0.6985. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.863
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.283
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         14354
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.283
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0118P)^2^+22.6686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1135
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12956
_reflns_number_total             14354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03114c2.cif
_cod_data_source_block           Turro2285
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               1559176
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.880
_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.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C21(H21), C22(H22), C23(H23), C24(H24),
  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),
  C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62)
2.b Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C2S(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              2750
_shelx_fab_checksum              13751
_olex2_submission_special_instructions 'No special instructions were received'