Metalla-phenalene complexes: synthesis, structure and aromaticity
Sun, Yue; Zhou, Yan; Bai, Wei; Yang, Li; Wang, Yilun; Chemical Communications  (2021) –; doi:10.1039/D1CC05855J

data_7129336
_publ_section_title
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 Metalla-phenalene complexes: synthesis, structure and aromaticity
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05855J
_journal_year                    2021
_chemical_formula_moiety         'C39 H34 Cl3 O P2 Re, 2(C H2 Cl2)'
_chemical_formula_sum            'C41 H38 Cl7 O P2 Re'
_chemical_formula_weight         1043.00
_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     direct
_audit_creation_date             2021-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-30 deposited with the CCDC.	2021-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.488(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7012(11)
_cell_length_b                   10.5762(10)
_cell_length_c                   36.545(4)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.79
_cell_measurement_theta_min      2.23
_cell_volume                     4123.4(7)
_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      120.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0981
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            69348
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.236
_exptl_absorpt_coefficient_mu    3.511
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       rod
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.145
_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     471
_refine_ls_number_reflns         9000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0242P)^2^+1.2248P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6668
_reflns_number_total             9000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05855j2.cif
_cod_data_source_block           baiwei14
_cod_database_code               7129336
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.720
_shelx_estimated_absorpt_t_min   0.474
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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:
 C1(H1), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
 C37(H37), C38(H38), C39(H39)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              52713
_olex2_submission_special_instructions 'No special instructions were received'