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_7131409
_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 O3 Os P3, Cl, 3(C H2 Cl2)'
_chemical_formula_sum            'C73 H69 Cl8 N2 O3 Os P3'
_chemical_formula_weight         1589.01
_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             2022-06-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-03-05 deposited with the CCDC.	2023-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.951(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9751(11)
_cell_length_b                   20.5087(17)
_cell_length_c                   26.253(2)
_cell_measurement_reflns_used    8337
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      67.08
_cell_measurement_theta_min      3.43
_cell_volume                     6858.8(10)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0463
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            54402
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.074
_diffrn_reflns_theta_max         67.074
_diffrn_reflns_theta_min         2.753
_diffrn_source_current           1.11
_diffrn_source_power             0.0555
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.431
_exptl_absorpt_correction_T_max  0.1642
_exptl_absorpt_correction_T_min  0.0549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1124 before and 0.0591 after correction.
The Ratio of minimum to maximum transmission is 0.3343.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       block
_exptl_crystal_F_000             3208
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.534
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         11981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+8.9174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11686
_reflns_number_total             11981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00029j2.cif
_cod_data_source_block           czw_mr_111_8_20220611_0m
_cod_depositor_comments
'Adding full bibliography for 7131403--7131410.cif.'
_cod_original_cell_volume        6858.9(10)
_cod_database_code               7131409
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.524
_shelx_estimated_absorpt_t_min   0.383
_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.a Ternary CH refined with riding coordinates:
 C00Q(H00Q)
2.b Secondary CH2 refined with riding coordinates:
 C01N(H01B,H01E), C02C(H02Q,H02R), C02D(H02M,H02N), C02F(H02G,H02H), C02H(H02O,
 H02P)
2.c Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N), C00P(H00P),
 C00R(H00R), C00U(H00U), C00X(H00X), C00Z(H00Z), C010(H010), C013(H013),
 C015(H015), C016(H016), C017(H017), C019(H019), C01A(H01A), C01C(H01C),
 C01D(H01D), C01F(H01F), C01G(H01G), C01H(H01H), C01J(H01J), C01K(H01K),
 C01L(H01L), C01M(H01M), C01O(H01O), C01P(H01P), C01Q(H01Q), 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), C025(H025), C026(H026), C027(H027), C028(H028), C02A(H02D),
 C02B(H02E), C02E(H02F), C02G(H02I)
2.d Idealised Me refined as rotating group:
 C029(H02A,H02B,H02C), C02I(H02J,H02K,H02L)
2.e Idealised tetrahedral OH refined as rotating group:
 O00D(H00D)
;
_shelx_res_checksum              62109
_shelx_hkl_checksum              48622
_olex2_submission_special_instructions 'No special instructions were received'