Preparation and Reactivity of Rhodium and Iridium Complexes Containing a Methylborohydride Based Unit Supported by Two 7-Azaindolyl Heterocycles
Da Costa, Rosenildo Correa; Rawe, Benjamin W.; Tsoureas, Nikolaos; Haddow, Mairi F.; Sparkes, Hazel Anne; Tizzard, Graham J.; Coles, Simon; Owen, Gareth Richard; Dalton Transactions  (2018) –; doi:10.1039/C8DT02311E

data_7047068
_publ_section_title
;
 Preparation and Reactivity of Rhodium and Iridium Complexes Containing a
 Methylborohydride Based Unit Supported by Two 7-Azaindolyl Heterocycles
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT02311E
_journal_year                    2018
_chemical_formula_moiety         'C23 H26 B N4 Rh'
_chemical_formula_sum            'C23 H26 B N4 Rh'
_chemical_formula_weight         472.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-06-05 deposited with the CCDC.
2018-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                111.4750(10)
_cell_angle_beta                 107.6280(10)
_cell_angle_gamma                106.4890(10)
_cell_formula_units_Z            6
_cell_length_a                   14.9965(3)
_cell_length_b                   16.0602(3)
_cell_length_c                   16.3753(5)
_cell_measurement_reflns_used    9086
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.61
_cell_volume                     3132.32(14)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_device_type  'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            87639
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.531
_diffrn_reflns_theta_min         1.520
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  0.7142
_exptl_absorpt_correction_T_min  0.6665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0459 before and 0.0406 after correction.
The Ratio of minimum to maximum transmission is 0.9332.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       block
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.402
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         14384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0342P)^2^+3.5312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12529
_reflns_number_total             14384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02311e2.cif
_cod_data_source_block           2_sq
_cod_original_cell_volume        3132.31(13)
_cod_database_code               7047068
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1), C16(H16), C17(H17), C20(H20), C21(H21), B2(H2), C39(H39), C40(H40),
 C43(H43), C44(H44), B3(H3A), C62(H62), C63(H63), C66(H66), C67(H67)
2.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C22(H22A,H22B), C23(H23A,H23B), C41(H41A,
 H41B), C42(H42A,H42B), C45(H45A,H45B), C46(H46A,H46B), C64(H64A,H64B),
 C65(H65A,H65B), C68(H68A,H68B), C69(H69A,H69B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C33(H33),
  C34(H34), C36(H36), C37(H37), C38(H38), C49(H49), C50(H50), C52(H52),
 C53(H53), C54(H54), C56(H56), C57(H57), C59(H59), C60(H60), C61(H61)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C24(H24A,H24B,H24C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              26308
_shelx_fab_checksum              25422
_olex2_submission_special_instructions 'No special instructions were received'