Sterically hindered Re- and Mn-CO<sub>2</sub> reduction catalysts for solar energy conversion.
Shipp, James D.; Carson, Heather; Spall, Steven J. P.; Parker, Simon C.; Chekulaev, Dimitri; Jones, Natalie; Mel'nikov, Mikhail Ya; Robertson, Craig C.; Meijer, Anthony J. H. M.; Weinstein, Julia A.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4230–4243; doi:10.1039/d0dt00252f

data_7703566
_publ_section_title
;
 Sterically hindered Re- and Mn-CO<sub>2</sub> reduction catalysts for
 solar energy conversion.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4230
_journal_page_last               4243
_journal_paper_doi               10.1039/d0dt00252f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C43 H50 Cl N4 O5 Re, C4 H10 O'
_chemical_formula_sum            'C47 H60 Cl N4 O6 Re'
_chemical_formula_weight         998.64
_chemical_name_common
'6,6?-{N(4-hexylphenyl)-N(ethyl)-amido}-2,2?-bipyridyl tricarbonylchlororhenium'
_chemical_name_systematic        '[Re(HPEAB)(CO)3Cl]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-24 deposited with the CCDC.	2020-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.5280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9608(5)
_cell_length_b                   16.3375(4)
_cell_length_c                   17.8363(5)
_cell_measurement_reflns_used    9759
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.80
_cell_measurement_theta_min      2.90
_cell_volume                     4435.0(2)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            68588
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.854
_diffrn_reflns_theta_max         66.854
_diffrn_reflns_theta_min         3.751
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.333
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/3 (Bruker,2014/3) was used for absorption correction. wR2(int) was 0.1222 before and 0.0723 after correction. The Ratio of minimum to maximum transmission is 0.5994. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       plate
_exptl_crystal_F_000             2040
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.695
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         7875
_refine_ls_number_restraints     555
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0576P)^2^+11.1528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6625
_reflns_number_total             7875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00252f2.cif
_cod_data_source_block           spall1_0m
_cod_depositor_comments
'Adding full bibliography for 7703566--7703567.cif.'
_cod_database_code               7703566
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.236
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 H20A-H22A
 2 with sigma of 0.02
 C12-C13B \\sim C12-C13A
 with sigma of 0.02
 C22B-C21 \\sim C22A-C21
 with sigma of 0.02
 C22B-C23B \\sim C23A-C22A
 with sigma of 0.02
 C23A-C24A \\sim C24B-C23B
 with sigma of 0.02
 C25B-C24B \\sim C25A-C24A
 with sigma of 0.02
 C36B-C35 \\sim C36A-C35
 with sigma of 0.02
 C37A-C36A \\sim C36B-C37B
 with sigma of 0.02
 C38A-C39A \\sim C39B-C38B
 with sigma of 0.02
 C45B-C44B \\sim C45A-C44A \\sim C47B-C46B \\sim C47A-C46A
 with sigma of 0.02
 O6B-C44B \\sim O6A-C44A \\sim O6B-C46B \\sim O6A-C46A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C13B) = Uanis(C13A)
Uanis(C25B) = Uanis(C24B) = Uanis(C23B) = Uanis(C22B)
Uanis(C22A) = Uanis(C23A) = Uanis(C24A) = Uanis(C25A)
Uanis(C45B) = Uanis(C44B) = Uanis(O6B) = Uanis(C46B) = Uanis(C47B)
Uanis(C45A) = Uanis(C44A) = Uanis(O6A) = Uanis(C46A) = Uanis(C47A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H21C)=Sof(H21D)=Sof(C22B)=Sof(H22C)=Sof(H22D)=Sof(C23B)=Sof(H23C)=
 Sof(H23D)=Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(C25B)=Sof(H25D)=Sof(H25E)=
 Sof(H25F)=1-FVAR(1)
 Sof(H21A)=Sof(H21B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(C23A)=Sof(H23A)=
 Sof(H23B)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(C25A)=Sof(H25A)=Sof(H25B)=
 Sof(H25C)=FVAR(1)
 Sof(H12C)=Sof(H12D)=Sof(C13B)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(H35C)=
 Sof(H35D)=Sof(C36B)=Sof(H36C)=Sof(H36D)=Sof(C37B)=Sof(H37C)=Sof(H37D)=
 Sof(C38B)=Sof(H38C)=Sof(H38D)=Sof(C39B)=Sof(H39C)=Sof(H39D)=Sof(H40D)=
 Sof(H40E)=Sof(H40F)=1-FVAR(2)
 Sof(H12A)=Sof(H12B)=Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(H35A)=
 Sof(H35B)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(C37A)=Sof(H37A)=Sof(H37B)=
 Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(C39A)=Sof(H39A)=Sof(H39B)=Sof(H40A)=
 Sof(H40B)=Sof(H40C)=FVAR(2)
 Sof(O6B)=Sof(C44B)=Sof(H44A)=Sof(H44B)=Sof(C45B)=Sof(H45A)=Sof(H45B)=
 Sof(H45C)=Sof(C46B)=Sof(H46A)=Sof(H46B)=Sof(C47B)=Sof(H47A)=Sof(H47B)=
 Sof(H47C)=1-FVAR(3)
 Sof(O6A)=Sof(C44A)=Sof(H44C)=Sof(H44D)=Sof(C45A)=Sof(H45D)=Sof(H45E)=
 Sof(H45F)=Sof(C46A)=Sof(H46C)=Sof(H46D)=Sof(C47A)=Sof(H47D)=Sof(H47E)=
 Sof(H47F)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C12(H12C,H12D), C12(H12A,H12B), C20(H20A,H20B), C21(H21C,H21D), C21(H21A,
 H21B), C22A(H22A,H22B), C22B(H22C,H22D), C23A(H23A,H23B), C23B(H23C,H23D),
 C24A(H24A,H24B), C24B(H24C,H24D), C27(H27A,H27B), C35(H35A,H35B), C35(H35C,
 H35D), C36A(H36A,H36B), C36B(H36C,H36D), C37A(H37A,H37B), C37B(H37C,H37D),
 C38A(H38A,H38B), C38B(H38C,H38D), C39A(H39A,H39B), C39B(H39C,H39D), C44A(H44C,
 H44D), C44B(H44A,H44B), C46A(H46C,H46D), C46B(H46A,H46B)
6.b Me refined with riding coordinates:
 C45B(H45A,H45B,H45C)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C15(H15), C16(H16), C18(H18),
 C19(H19), C30(H30), C31(H31), C33(H33), C34(H34)
6.d Idealised Me refined as rotating group:
 C13A(H13A,H13B,H13C), C13B(H13D,H13E,H13F), C25A(H25A,H25B,H25C), C25B(H25D,
 H25E,H25F), C28(H28A,H28B,H28C), C40(H40A,H40B,H40C), C40(H40D,H40E,H40F),
 C45A(H45D,H45E,H45F), C47A(H47D,H47E,H47F), C47B(H47A,H47B,H47C)
;
_shelx_res_checksum              89410
_olex2_submission_special_instructions 'No special instructions were received'