Synthesis of tricyclic 1,4-dihydro-1,4-phosphagermines - trying to establish molecular fencing of reactive centers.
Ramachandran, Mridhul R. K.; Karwasara, Surendar; Zhu, Hui; Schnakenburg, Gregor; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7953–7957; doi:10.1039/d4dt00895b

data_7715765
_publ_section_title
;
 Synthesis of tricyclic 1,4-dihydro-1,4-phosphagermines - trying to
 establish molecular fencing of reactive centers.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7953
_journal_page_last               7957
_journal_paper_doi               10.1039/d4dt00895b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '2(C18 H34 Ge N6 S2), C4 H10 O'
_chemical_formula_sum            'C40 H78 Ge2 N12 O S4'
_chemical_formula_weight         1016.56
_chemical_name_systematic        MR-391
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-02-01 deposited with the CCDC.	2024-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                75.118(4)
_cell_angle_beta                 72.831(5)
_cell_angle_gamma                81.836(5)
_cell_formula_units_Z            2
_cell_length_a                   10.4910(7)
_cell_length_b                   15.5099(8)
_cell_length_c                   17.3593(10)
_cell_measurement_reflns_used    47951
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.25
_cell_measurement_theta_min      4.41
_cell_volume                     2601.5(3)
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)'
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            56715
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         67.734
_diffrn_reflns_theta_min         4.423
_diffrn_source                   'Axo Cu'
_exptl_absorpt_coefficient_mu    3.251
_exptl_absorpt_correction_T_max  0.4835
_exptl_absorpt_correction_T_min  0.2573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         9314
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0545
_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^)+(0.1021P)^2^+2.2668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7130
_reflns_number_total             9314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00895b2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7715765--7715769.cif.'
_cod_database_code               7715765
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.356
_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. Restrained distances
 C18S-C17S
 1.5 with sigma of 0.01
3. Rigid bond restraints
 N6A, C17S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C17S) \\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C18S) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Sof(C17S)=Sof(H17C)=Sof(H17D)=Sof(C18S)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(1)
 Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C11(H11C,H11D), C13(H13C,H13D), C15(H15C,H15D), C17(H17E,H17F), C11A(H11A,
 H11B), C13A(H13A,H13B), C15A(H15A,H15B), C17A(H17A,H17B), C17S(H17C,H17D),
 C20(H20A,H20B), C21(H21A,H21B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C3A(H3A), C8A(H8A)
6.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C10(H10D,H10E,H10F),
 C12(H12D,H12E,H12F), C14(H14D,H14E,H14F), C16(H16D,H16E,H16F), C18(H18G,H18H,
 H18I), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC), C9A(H9AA,H9AB,H9AC),
 C10A(H10A,H10B,H10C), C12A(H12A,H12B,H12C), C14A(H14A,H14B,H14C), C16A(H16A,
 H16B,H16C), C18A(H18A,H18B,H18C), C18S(H18D,H18E,H18F), C19(H19A,H19B,H19C),
 C22(H22A,H22B,H22C)
;
_shelx_res_checksum              53362
_olex2_submission_special_instructions 'No special instructions were received'