One-pot syntheses of irida-polycyclic aromatic hydrocarbons
Hu, Yuxuan; Zhang, Jing; Wang, Xiaoyan; Lu, Zhengyu; Zhang, Fangfang; Yang, Xiaofei; Ma, Zhihua; Yin, Jun; Xia, Haiping; Liu, Shenghua; Chemical Science  (2019) –; doi:10.1039/C9SC03914G

data_1552424
_publ_section_title
;
 One-pot syntheses of irida-polycyclic aromatic hydrocarbons
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC03914G
_journal_year                    2019
_chemical_formula_moiety         'C29 H35 Ir O P, C24 H20 B'
_chemical_formula_sum            'C53 H55 B Ir O P'
_chemical_formula_weight         941.95
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2019-07-15
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-15 deposited with the CCDC.    2019-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.492(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.264(6)
_cell_length_b                   16.108(7)
_cell_length_c                   18.770(7)
_cell_measurement_reflns_used    5460
_cell_measurement_temperature    295
_cell_measurement_theta_max      55.30
_cell_measurement_theta_min      3.33
_cell_volume                     4447(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 0.921
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12386
_diffrn_reflns_point_group_measured_fraction_full 0.921
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        55.294
_diffrn_reflns_theta_max         55.294
_diffrn_reflns_theta_min         4.315
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.424
_exptl_absorpt_correction_T_max  0.7509
_exptl_absorpt_correction_T_min  0.5007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1445 before and 0.0685 after correction. The Ratio of minimum to maximum transmission is 0.6668. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'metallic black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       plate
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         5199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0324P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4583
_reflns_number_total             5199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc03914g2.cif
_cod_data_source_block           Complex_1
_cod_database_code               1552424
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.446
_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), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C15(H15),
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39),
  C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47),
 C49(H49), C50(H50), C51(H51), C52(H52), C53(H53)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              86349
_olex2_submission_special_instructions 'No special instructions were received'