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_7131408
_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         '2(C66 H53 N2 O Os P3), 4(F6 Sb), C H2 Cl2'
_chemical_formula_sum            'C133 H108 Cl2 F24 N4 O2 Os2 P6 Sb4'
_chemical_formula_weight         3374.35
_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                104.879(4)
_cell_angle_beta                 91.321(4)
_cell_angle_gamma                95.310(4)
_cell_formula_units_Z            2
_cell_length_a                   11.6995(9)
_cell_length_b                   21.8835(15)
_cell_length_c                   25.5349(19)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.33
_cell_measurement_theta_min      3.80
_cell_volume                     6283.8(8)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_collection       'Apex3 (Bruker 2018)'
_computing_data_reduction        'SAINT V8.40A (?, 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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0819
_diffrn_reflns_av_unetI/netI     0.0963
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            75780
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        62.496
_diffrn_reflns_theta_max         62.496
_diffrn_reflns_theta_min         2.100
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.319
_exptl_absorpt_correction_T_max  0.1665
_exptl_absorpt_correction_T_min  0.0516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1529 before and 0.0927 after correction.
The Ratio of minimum to maximum transmission is 0.3099.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'yellowish green'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_description       block
_exptl_crystal_F_000             3292
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.900
_refine_diff_density_min         -1.662
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1657
_refine_ls_number_reflns         19902
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+8.1822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14923
_reflns_number_total             19902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00029j2.cif
_cod_data_source_block           czw508_20210428_0m
_cod_depositor_comments
'Adding full bibliography for 7131403--7131410.cif.'
_cod_database_code               7131408
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.525
_shelx_estimated_absorpt_t_min   0.320
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
F2 \\sim Sb1 \\sim F3 \\sim F4 \\sim F8 \\sim F1AA \\sim F11 \\sim F2AA \\sim
Sb0A \\sim F7 \\sim F18 \\sim F5 \\sim F0AA \\sim F9: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: Sb1(0.5) Sb0A(0.5) F2(0.5) F3(0.5) F4(0.5) F5(0.5) F7(0.5) F8(0.5)
 F1AA(0.5) F0AA(0.5) F9(0.5) F11(0.5) F18(0.5) F2AA(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C04X(H04T,H04V)
4.b Aromatic/amide H refined with riding coordinates:
 C00X(H00X), C013(H013), C014(H014), C015(H015), C01A(H01A), C01B(H01B),
 C01E(H01E), C01F(H01F), C01G(H01G), C01H(H01H), C01K(H01K), C01L(H01L),
 C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), C01U(H01U),
 C01W(H01W), C01Z(H01Z), C020(H020), C021(H021), C022(H022), C023(H023),
 C024(H024), C025(H025), C027(H027), C028(H028), C029(H029), C02A(H02A),
 C02B(H02B), C02C(H02C), C02D(H02D), C02E(H02E), C02F(H02F), C02G(H02G),
 C02H(H02H), C02I(H02I), C02J(H02J), C02M(H02M), C02N(H02N), C02O(H02O),
 C02R(H02R), C02S(H02S), C02T(H02T), C02U(H02U), C02V(H02V), C02Y(H02Y),
 C02Z(H02Z), C030(H030), C031(H031), C032(H032), C033(H033), C034(H034),
 C035(H035), C037(H037), C038(H038), C039(H039), C03B(H03B), C03C(H03C),
 C03D(H03D), C03E(H03E), C03F(H03F), C03G(H03G), C03H(H03H), C03I(H03I),
 C03J(H03J), C03M(H03M), C03P(H03P), C03Q(H03Q), C03S(H03S), C03T(H03T),
 C03U(H03U), C03V(H03V), C03X(H03X), C03Y(H03Y), C03Z(H03Z), C040(H040),
 C041(H041), C042(H042), C044(H044), C045(H045), C046(H046), C047(H047),
 C048(H048), C049(H049), C04A(H04A), C04B(H04B), C04C(H04C), C04D(H04D),
 C04E(H04E), C04F(H04F), C04G(H04G), C04H(H04H), C04I(H04I), C04J(H04J),
 C04K(H04K), C04L(H04L), C04M(H04M), C04N(H04N), C04O(H04O), C04P(H04P),
 C04Q(H04Q), C04R(H04R), C04S(H04S), C04U(H04U)
;
_shelx_res_checksum              40954
_shelx_hkl_checksum              70659
_olex2_submission_special_instructions 'No special instructions were received'