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_7131403
_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         'C69 H61 Cl N2 O3 Os P3, Cl, 3.5(C H2 Cl2)'
_chemical_formula_sum            'C72.5 H68 Cl9 N2 O3 Os P3'
_chemical_formula_weight         1617.44
_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     dual
_audit_creation_date             2023-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-03-06 deposited with the CCDC.	2023-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.736(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1837(3)
_cell_length_b                   20.2111(5)
_cell_length_c                   26.5287(7)
_cell_measurement_reflns_used    9022
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      69.28
_cell_measurement_theta_min      2.76
_cell_volume                     6986.8(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_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_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  0.0524
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            75298
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.589
_diffrn_reflns_theta_min         2.760
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.650
_exptl_absorpt_correction_T_max  0.2094
_exptl_absorpt_correction_T_min  0.0891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1693 before and 0.0661 after correction.
The Ratio of minimum to maximum transmission is 0.4255.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       block
_exptl_crystal_F_000             3260
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.640
_refine_diff_density_min         -1.233
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     921
_refine_ls_number_reflns         12963
_refine_ls_number_restraints     163
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+57.6488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1510
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11183
_reflns_number_total             12963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00029j2.cif
_cod_data_source_block           czw_20230303_0m
_cod_depositor_comments
'Adding full bibliography for 7131403--7131410.cif.'
_cod_original_formula_sum        'C72.50 H68 Cl9 N2 O3 Os P3'
_cod_database_code               7131403
_shelx_shelxl_version_number     2018/3
_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, All O(H) groups
2. Restrained distances
 O00H-C11
 1.42 with sigma of 0.02
 C4-C11 = C4-C2
 1.54 with sigma of 0.02
 O36-C9
 1.42 with sigma of 0.02
 Cl0C-C3 = Cl-C3 = Cl09-C02D = Cl0B-C02D
 1.79 with sigma of 0.02
 Cl7-C5 = Cl3-C18 = Cl5-C31 = Cl8-C5 = Cl1-C18 = Cl6-C31
 1.79 with sigma of 0.02
 C6-C34 = C35-C34
 1.54 with sigma of 0.02
 C9-C32 = C33-C32
 1.54 with sigma of 0.02
 O36-C6
 1.42 with sigma of 0.02
 C11-C2
 2.53 with sigma of 0.04
 Cl6-Cl1 = Cl8-Cl7
 2.9 with sigma of 0.04
 C6-C35
 2.53 with sigma of 0.04
 C9-C33
 2.53 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C9 \\sim C32 \\sim C33 \\sim C6 \\sim C34 \\sim C35 \\sim C2 \\sim C4 \\sim C11
\\sim O00H \\sim O36 \\sim C025: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cl0B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl0B) = Uanis(Cl0C)
Uanis(C02D) = Uanis(C3)
Uanis(Cl09) = Uanis(Cl)
Uanis(Cl7) = Uanis(Cl3) = Uanis(Cl5)
Uanis(Cl8) = Uanis(Cl1) = Uanis(Cl6)
Uanis(C5) = Uanis(C18) = Uanis(C31)
4. Others
 1*[Sof(Cl1)+Sof(Cl3)+Sof(C18)+Sof(H18A)+Sof(H18B)]+1*[Sof(Cl5)+Sof(Cl6)+
 Sof(C31)+Sof(H31A)+Sof(H31B)]+1*[Sof(Cl8)+Sof(Cl7)+Sof(C5)+Sof(H5A)+Sof(H5B)]=
 1 with esd of 0
 1*[Sof(C4)+Sof(H4A)+Sof(H4B)+Sof(C2)+Sof(H2A)+Sof(H2B)+Sof(H2C)+Sof(C11)+
 Sof(H11A)+Sof(H11B)]+1*[Sof(C9)+Sof(H9A)+Sof(H9B)+Sof(C32)+Sof(H32A)+Sof(H32B)+
 Sof(C33)+Sof(H33A)+Sof(H33B)+Sof(H33C)]+1*[Sof(C6)+Sof(H6A)+Sof(H6B)+Sof(C35)+
 Sof(H35A)+Sof(H35B)+Sof(H35C)+Sof(C34)+Sof(H34A)+Sof(H34B)]=1 with esd of 0
 Sof(Cl1)=Sof(Cl3)=Sof(C18)=Sof(H18A)=Sof(H18B)=FVAR(1)
 Sof(Cl)=Sof(Cl0C)=Sof(C3)=Sof(H3A)=Sof(H3B)=1-FVAR(2)
 Sof(Cl09)=Sof(Cl0B)=Sof(C02D)=Sof(H02D)=Sof(H02G)=FVAR(2)
 Sof(Cl5)=Sof(Cl6)=Sof(C31)=Sof(H31A)=Sof(H31B)=FVAR(3)
 Sof(Cl8)=Sof(Cl7)=Sof(C5)=Sof(H5A)=Sof(H5B)=FVAR(4)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C11)=
 Sof(H11A)=Sof(H11B)=FVAR(5)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C33)=Sof(H33A)=
 Sof(H33B)=Sof(H33C)=FVAR(6)
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C34)=
 Sof(H34A)=Sof(H34B)=FVAR(7)
 Fixed Sof: Cl2(0.5) Cl4(0.5) C1(0.5) H1A(0.5) H1B(0.5)
5.a Ternary CH refined with riding coordinates:
 C00L(H00L)
5.b Secondary CH2 refined with riding coordinates:
 C01N(H01A,H01E), C02D(H02D,H02G), C1(H1A,H1B), C9(H9A,H9B), C18(H18A,H18B),
 C4(H4A,H4B), C11(H11A,H11B), C3(H3A,H3B), C5(H5A,H5B), C31(H31A,H31B), C6(H6A,
 H6B), C32(H32A,H32B), C34(H34A,H34B)
5.c Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00G(H00G), C00K(H00K), C00O(H00O), C00V(H00V), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C011(H011), C012(H012), C013(H013),
 C014(H014), C015(H015), C016(H016), C018(H018), C019(H019), C01B(H01B),
 C01C(H01C), C01D(H01D), C01F(H01F), C01G(H01G), C01H(H01H), C01I(H01I),
 C01J(H01J), C01L(H01L), C01M(H01M), C01O(H01O), C01P(H01P), C01R(H01R),
 C01S(H01S), C01T(H01T), C01U(H01U), C01V(H01V), C01W(H01W), C01X(H01X),
 C01Y(H01Y), C01Z(H01Z), C020(H020), C021(H021), C022(H022), C023(H023),
 C024(H024), C026(H026), C027(H027), C028(H028), C029(H029), C02A(H02A),
 C02B(H02B), C02C(H02C), C02E(H02E), C02F(H02F)
5.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C35(H35A,H35B,H35C), C33(H33A,H33B,H33C)
5.e Idealised tetrahedral OH refined as rotating group:
 O00C(H00C)
;
_shelx_res_checksum              52958
_shelx_hkl_checksum              76414
_olex2_submission_special_instructions 'No special instructions were received'