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_7715769
_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         'C43 H46 Cl Ge N4 P S2, 2(C4 H8 O)'
_chemical_formula_sum            'C51 H62 Cl Ge N4 O2 P S2'
_chemical_formula_weight         966.17
_chemical_name_systematic        SKARR-18
_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             2023-04-17
_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                70.439(7)
_cell_angle_beta                 78.468(6)
_cell_angle_gamma                66.212(7)
_cell_formula_units_Z            2
_cell_length_a                   13.9471(11)
_cell_length_b                   14.1197(13)
_cell_length_c                   14.5100(12)
_cell_measurement_reflns_used    6748
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.08
_cell_measurement_theta_min      3.47
_cell_volume                     2456.8(4)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.189.0 (STOE, 2022)
;
_computing_data_reduction
;
X-Area Integrate 2.5.11.0 (STOE, 2022)
X-Area LANA 2.7.9.0 (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      100.15
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
 2359 frames, detector distance = 40 mm

Twin law determined via inspection of the reciprocal space-group    
Twin law for transforming hkl(1) to hkl(2):    1.01345 -0.00596 -0.05248
                                               0.02141  0.98750  0.01575
                                               0.07359 -0.04353  0.99736
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_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_unetI/netI     0.5668
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            113633
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         67.748
_diffrn_reflns_theta_min         3.567
_exptl_absorpt_coefficient_mu    2.782
_exptl_absorpt_correction_T_max  0.6334
_exptl_absorpt_correction_T_min  0.1228
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.387
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         113633
_refine_ls_number_restraints     525
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.3739
_refine_ls_R_factor_gt           0.1397
_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^)+(0.1298P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3069
_refine_ls_wR_factor_ref         0.4121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26684
_reflns_number_total             113633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00895b2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7715765--7715769.cif.'
_cod_database_code               7715769
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.697
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.586(3)
 0.414(3)
2. 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
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,
 H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B)
4.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C18(H18), C20(H20), C27(H27), C29(H29), C36(H36), C38(H38)
4.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C)
;
_shelx_res_checksum              25570
_olex2_submission_special_instructions 'No special instructions were received'