Hetero-carbolong chemistry: experimental and theoretical studies of diaza-metallapentalenes.
Chu, Zhenwei; Li, Jinhua; Hua, Yuhui; Luo, Ming; Chen, Dafa; Xia, Haiping; Chemical communications (Cambridge, England) 59 (2023) 4173–4176; doi:10.1039/d3cc00029j

data_7131410
_publ_section_title
;
 Hetero-carbolong chemistry: experimental and theoretical studies of
 diaza-metallapentalenes.
;
_journal_issue                   28
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4173
_journal_page_last               4176
_journal_paper_doi               10.1039/d3cc00029j
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C67 H55 N2 O Os P3, 2(F6 Sb), 2(C H2 Cl2)'
_chemical_formula_sum            'C69 H59 Cl4 F12 N2 O Os P3 Sb2'
_chemical_formula_weight         1828.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-12-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-03-05 deposited with the CCDC.	2023-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                81.356(2)
_cell_angle_beta                 78.117(2)
_cell_angle_gamma                84.437(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1145(5)
_cell_length_b                   13.6851(6)
_cell_length_c                   23.2566(10)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      52.95
_cell_measurement_theta_min      2.85
_cell_volume                     3414.3(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Apex3 (Bruker 2018)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            67848
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        52.981
_diffrn_reflns_theta_max         52.981
_diffrn_reflns_theta_min         1.704
_exptl_absorpt_coefficient_mu    8.436
_exptl_absorpt_correction_T_max  0.7505
_exptl_absorpt_correction_T_min  0.5991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1132 before and 0.0647 after correction.
The Ratio of minimum to maximum transmission is 0.7983.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       block
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.246
_refine_diff_density_min         -1.783
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         12009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0419P)^2^+10.4549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10818
_reflns_number_total             12009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00029j2.cif
_cod_data_source_block           czw_20221102_2_0m
_cod_depositor_comments
'Adding full bibliography for 7131403--7131410.cif.'
_cod_database_code               7131410
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.632
_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. Uiso/Uaniso restraints and constraints
Uanis(C17) = Uanis(C02L) = Uanis(C02K) = Uanis(C9) = Uanis(C16) = Uanis(C02F) =
Uanis(C02E) = Uanis(C38) = Uanis(C35) = Uanis(C02A) = Uanis(C01Z)
Uanis(C1) = Uanis(C021) = Uanis(C2) = Uanis(C18) = Uanis(C3AA) = Uanis(C7) =
Uanis(C5) = Uanis(C6) = Uanis(C2AA) = Uanis(C8)
Uanis(C02H) = Uanis(C02G) = Uanis(C1AA) = Uanis(C027) = Uanis(C01T) =
Uanis(C018) = Uanis(C022) = Uanis(C10)
Uanis(C02M) = Uanis(C0AA) = Uanis(Cl0A) = Uanis(Cl7) = Uanis(Cl09) = Uanis(Cl5)
3. Others
 Fixed Sof: Cl09(0.5) Cl0A(0.5) H027(0.5) H02D(0.5) C02A(0.5) H02E(0.5)
 C02E(0.5) H02F(0.5) C02F(0.66667) H02G(0.66667) C02G(0.5) H02H(0.5) C02H(0.5)
 H02I(0.5) C02K(0.66667) H02K(0.66667) C02L(0.66667) H02L(0.66667) C02M(0.5)
 H02N(0.5) H02O(0.5) C9(0.33333) H9(0.33333) C16(0.33333) H16(0.33333)
 C17(0.33333) H17(0.33333) C35(0.5) H35(0.5) C38(0.5) H38(0.5) Cl5(0.5)
 Cl7(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5) H1A(0.5) H1B(0.5) C2(0.5) H2(0.5)
 C7(0.5) H7(0.5) C8(0.5) H8(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5) C3AA(0.5)
 H3AA(0.5) C1AA(0.5) H1AA(0.5) C10(0.5) H10(0.5) C2AA(0.5) H2AA(0.5) C18(0.5)
 H18(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C02B(H02J,H02M), C02M(H02N,H02O), C0AA(H0AA,H0AB)
4.b Aromatic/amide H refined with riding coordinates:
 C00R(H00R), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X),
 C010(H010), C011(H011), C012(H012), C013(H013), C014(H014), C016(H016),
 C018(H018), C019(H019), C01A(H01A), C01B(H01B), C01C(H01C), C01D(H01D),
 C01E(H01E), C01F(H01F), C01G(H01G), C01H(H01H), C01J(H01J), C01L(H01L),
 C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), C01R(H01R),
 C01S(H01S), C01T(H01T), C01U(H01U), C01V(H01V), C01W(H01W), C023(H023),
 C025(H025), C027(H027), C027(H02D), C028(H028), C029(H029), C02A(H02E),
 C02E(H02F), C02F(H02G), C02G(H02H), C02H(H02I), C02K(H02K), C02L(H02L), C9(H9),
  C16(H16), C17(H17), C35(H35), C38(H38), C1(H1A), C1(H1B), C2(H2), C7(H7),
 C8(H8), C5(H5), C6(H6), C3AA(H3AA), C1AA(H1AA), C10(H10), C2AA(H2AA), C18(H18)
4.c Idealised Me refined as rotating group:
 C026(H02A,H02B,H02C)
;
_shelx_res_checksum              81378
_shelx_hkl_checksum              21963
_olex2_submission_special_instructions 'No special instructions were received'