Photoswitchable hydride transfer from iridium to 1-methylnicotinamide rationalized by thermochemical cycles.
Barrett, Seth M.; Pitman, Catherine L.; Walden, Andrew G.; Miller, Alexander J. M.; Journal of the American Chemical Society 136 (2014) 14718–14721; doi:10.1021/ja508762g

data_4122782
_publ_section_title
;
 Photoswitchable hydride transfer from iridium to 1-methylnicotinamide
 rationalized by thermochemical cycles.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14718
_journal_page_last               14721
_journal_paper_doi               10.1021/ja508762g
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C42 H50 Ir2 N5, 3(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C46 H56 F18 Ir2 N7 P3'
_chemical_formula_weight         1526.28
_chemical_name_systematic
;
 ?
;
_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     direct
_audit_creation_date             2014-08-15
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.1101(3)
_cell_length_b                   11.0118(2)
_cell_length_c                   19.22650(10)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.11
_cell_measurement_theta_min      3.52
_cell_volume                     5316.27(12)
_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, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.988
_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  0.0560
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            58370
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.117
_diffrn_reflns_theta_min         3.520
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.345
_exptl_absorpt_correction_T_max  0.6888
_exptl_absorpt_correction_T_min  0.2643
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1332 before and 0.0766 after correction.
The Ratio of minimum to maximum transmission is 0.3837.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_description       plate
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.087
_refine_diff_density_max         1.964
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.37(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         9803
_refine_ls_number_restraints     760
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+34.4268P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                8948
_reflns_number_total             9803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja508762g_si_002.cif
_cod_data_source_block           sb106_c
_cod_depositor_comments          'Adding full bibliography for 4122782.cif.'
_cod_database_code               4122782
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.439
_shelx_estimated_absorpt_t_min   0.152
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. 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
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C23(H23), C24(H24), C25(H25), C26(H26), C29(H29), C30(H30), C31(H31), C32(H32)
3.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C34(H34A,H34B,H34C), C36(H36A,
 H36B,H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C),
 C44(H44A,H44B,H44C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              46383
_shelx_hkl_checksum              37102
_olex2_submission_original_sample_id SB106
_olex2_submission_special_instructions 'No special instructions were received'