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_7131406
_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         'C70 H63 Cl N2 O4 Os P3, Cl, 3(C H2 Cl2)'
_chemical_formula_sum            'C73 H69 Cl8 N2 O4 Os P3'
_chemical_formula_weight         1605.01
_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             2022-10-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-02 deposited with the CCDC.	2023-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.668(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8076(5)
_cell_length_b                   20.4760(8)
_cell_length_c                   26.9271(10)
_cell_measurement_reflns_used    9631
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      66.63
_cell_measurement_theta_min      3.48
_cell_volume                     6998.4(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Apex3 (Bruker 2018)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2014'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'Bruker PHOTON II area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CMOS area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            61949
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.636
_diffrn_reflns_theta_max         66.636
_diffrn_reflns_theta_min         2.720
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.300
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0583 before and 0.0370 after correction.
The Ratio of minimum to maximum transmission is 0.8734.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.077
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         12350
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0209
_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^)+(0.0187P)^2^+8.6901P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0490
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11856
_reflns_number_total             12350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00029j2.cif
_cod_data_source_block           czw_mr_218_3_20221022_0m
_cod_depositor_comments
'Adding full bibliography for 7131403--7131410.cif.'
_cod_database_code               7131406
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.593
_shelx_estimated_absorpt_t_min   0.388
_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. Uiso/Uaniso restraints and constraints
Cl0C \\sim C02B \\sim Cl07: within 2A with sigma of 0.05 and sigma for terminal
atoms of 0.1 within 2A
Uanis(C02J) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C00N(H00N)
3.b Secondary CH2 refined with riding coordinates:
 C01R(H01A,H01D), C02A(H02P,H02Q), C02B(H02N,H02O), C02H(H02I,H02J), C02J(H02R,
 H02S)
3.c Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00K(H00K), C00M(H00M), C00Q(H00Q), C00R(H00R), C00T(H00T),
 C00U(H00U), C00W(H00W), C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011),
 C012(H012), C015(H015), C017(H017), C019(H019), C01B(H01B), C01C(H01C),
 C01F(H01F), C01G(H01G), C01H(H01H), C01I(H01I), C01K(H01K), C01L(H01L),
 C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), 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),
 C025(H025), C026(H026), C027(H027), C029(H029), C02C(H02D), C02D(H02E),
 C02E(H02F), C02F(H02G), C02G(H02H)
3.d Idealised Me refined as rotating group:
 C028(H02A,H02B,H02C), C02I(H02K,H02L,H02M)
3.e Idealised tetrahedral OH refined as rotating group:
 O00D(H00D)
;
_shelx_res_checksum              72327
_shelx_hkl_checksum              7017
_olex2_submission_special_instructions 'No special instructions were received'