A bis(germylene) functionalized metal-coordinated polyphosphide and its isomerization.
Yadav, Ravi; Goswami, Bhupendra; Simler, Thomas; Schoo, Christoph; Reichl, Stephan; Scheer, Manfred; Roesky, Peter W.; Chemical communications (Cambridge, England) 56 (2020) 10207–10210; doi:10.1039/d0cc03920a

data_7127008
_publ_section_title
;
 A bis(germylene) functionalized metal-coordinated polyphosphide and its
 isomerization.
;
_journal_issue                   70
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10207
_journal_page_last               10210
_journal_paper_doi               10.1039/d0cc03920a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C40 H61 Fe Ge2 N4 P5, C7 H8'
_chemical_formula_sum            'C47 H69 Fe Ge2 N4 P5'
_chemical_formula_weight         1045.94
_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             2020-03-11
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2020-06-03 deposited with the CCDC.	2020-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                98.830(10)
_cell_angle_beta                 110.410(10)
_cell_angle_gamma                92.274(9)
_cell_formula_units_Z            2
_cell_length_a                   12.9054(14)
_cell_length_b                   13.5536(14)
_cell_length_c                   17.432(3)
_cell_measurement_reflns_used    24352
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      1.54
_cell_volume                     2809.5(7)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.127.0 (STOE, 2016)'
_computing_data_reduction
;
X-Area Integrate 1.71.0.0 (STOE, 2016)
X-Area X-Red32 1.63.2.0 (STOE, 2017)
;
_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 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.773
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0836
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.773
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26911
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.773
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.153
_diffrn_reflns_theta_min         1.711
_exptl_absorpt_coefficient_mu    1.492
_exptl_absorpt_correction_T_max  0.8993
_exptl_absorpt_correction_T_min  0.3913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
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.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       plate
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.964
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         14041
_refine_ls_number_restraints     468
_refine_ls_restrained_S_all      3.754
_refine_ls_R_factor_all          0.1253
_refine_ls_R_factor_gt           0.0679
_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^)+(0.0898P)^2^+2.3881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1873
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8228
_reflns_number_total             14041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03920a2.cif
_cod_data_source_block           ry448sv
_cod_depositor_comments
'Adding full bibliography for 7127008--7127009.cif.'
_cod_original_cell_volume        2809.5(6)
_cod_database_code               7127008
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.725
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C42A-C47A = C42A-C43A = C46A-C45A
 1.39 with sigma of 0.02
 C41A-C42A
 1.51 with sigma of 0.02
 C47A-C46A = C45A-C44A = C44A-C43A
 1.38 with sigma of 0.02
 C43B-C44B = C45B-C46B = C46B-C47B
 1.38 with sigma of 0.02
 C42B-C43B = C42B-C47B = C44B-C45B
 1.39 with sigma of 0.02
 C41B-C42B
 1.51 with sigma of 0.02
 C42A-C46A
 2.42 with sigma of 0.04
 C46A-C44A = C45A-C43A
 2.4 with sigma of 0.04
 C42A-C44A
 2.41 with sigma of 0.04
 C41A-C47A = C41A-C43A
 2.52 with sigma of 0.04
 C47A-C45A
 2.39 with sigma of 0.04
 C41B-C43B = C41B-C47B
 2.52 with sigma of 0.04
 C43B-C45B
 2.39 with sigma of 0.04
 C44B-C46B = C45B-C47B
 2.4 with sigma of 0.04
 C42B-C44B
 2.42 with sigma of 0.04
 C42B-C46B
 2.41 with sigma of 0.04
 C42A-C47A \\sim C47A-C46A \\sim C46A-C45A \\sim C45A-C44A \\sim C44A-C43A
\\sim C43A-C42A
 with sigma of 0.02
 C42A-C44A \\sim C42A-C46A \\sim C43A-C45A \\sim C47A-C43A \\sim C46A-C44A
\\sim C47A-C45A
 with sigma of 0.04
 C41A-C43A \\sim C41A-C47A
 with sigma of 0.04
 C33A-C32A \\sim C32A-C36A \\sim C36A-C35A \\sim C35A-C34A \\sim C34A-C33A
 with sigma of 0.02
 C33A-C36A \\sim C32A-C35A \\sim C36A-C34A \\sim C34A-C32A \\sim C33A-C35A
 with sigma of 0.04
 C33A-C38A \\sim C32A-C39A \\sim C36A-C40A \\sim C35A-C31A \\sim C34A-C37A
 with sigma of 0.02
 C38A-C32A \\sim C38A-C34A \\sim C39A-C33A \\sim C39A-C36A \\sim C40A-C32A
\\sim C40A-C35A \\sim C31A-
 C36A \\sim C31A-C34A \\sim C37A-C35A \\sim C37A-C33A
 with sigma of 0.04
 C42B-C46B \\sim C42B-C44B \\sim C47B-C45B \\sim C43B-C47B \\sim C44B-C46B
\\sim C43B-C45B
 with sigma of 0.04
 C42B-C43B \\sim C43B-C44B \\sim C44B-C45B \\sim C45B-C46B \\sim C46B-C47B
\\sim C47B-C42B
 with sigma of 0.02
 C41B-C47B \\sim C41B-C43B
 with sigma of 0.04
 C36B-C32B \\sim C32B-C33B \\sim C33B-C34B \\sim C34B-C35B \\sim C35B-C36B
 with sigma of 0.02
 C36B-C33B \\sim C32B-C34B \\sim C33B-C35B \\sim C35B-C32B \\sim C36B-C34B
 with sigma of 0.04
 C36B-C39B \\sim C32B-C38B \\sim C33B-C37B \\sim C34B-C31B \\sim C35B-C40B
 with sigma of 0.02
 C39B-C32B \\sim C39B-C35B \\sim C38B-C36B \\sim C38B-C33B \\sim C37B-C32B
\\sim C37B-C34B \\sim C31B-
 C33B \\sim C31B-C35B \\sim C40B-C34B \\sim C40B-C36B
 with sigma of 0.04
3. Restrained planarity
 C41A, C42A, C47A, C46A, C45A, C44A, C43A
 with sigma of 0.1
 C33A, C32A, C36A, C35A, C34A, C37A, C31A, C40A, C39A, C38A
 with sigma of 0.1
 C41B, C42B, C43B, C44B, C45B, C46B, C47B
 with sigma of 0.1
 C36B, C32B, C33B, C34B, C35B, C40B, C31B, C37B, C38B, C39B
 with sigma of 0.1
4. Rigid bond restraints
 C33A, C32A, C36A, C35A, C34A, C37A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14B, C13B, C15B, C14A, C15A, C13A, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C41A \\sim C42A \\sim C47A \\sim C46A \\sim C45A \\sim C44A \\sim C43A: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C33A \\sim C32A \\sim C36A \\sim C35A \\sim C34A \\sim C37A \\sim C31A \\sim
C40A \\sim C39A \\sim C38A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C41B \\sim C42B \\sim C43B \\sim C44B \\sim C45B \\sim C46B \\sim C47B: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C36B \\sim C32B \\sim C33B \\sim C34B \\sim C35B \\sim C40B \\sim C31B \\sim
C37B \\sim C38B \\sim C39B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
: with sigma of 0.1 and sigma for terminal atoms of 0.2
6. Rigid body (RIGU) restrains
 C41A, C42A, C47A, C46A, C45A, C44A, C43A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C33A, C32A, C36A, C35A, C34A, C37A, C31A, C40A, C39A, C38A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41B, C42B, C43B, C44B, C45B, C46B, C47B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C36B, C32B, C33B, C34B, C35B, C40B, C31B, C37B, C38B, C39B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: C41A(0.65) H1A(0.65) H1B(0.65) H1C(0.65) C42A(0.65) C47A(0.65)
 H13(0.65) C46A(0.65) H14(0.65) C45A(0.65) H15(0.65) C44A(0.65) H16(0.65)
 C43A(0.65) H17(0.65) C41B(0.35) H41A(0.35) H41B(0.35) H41C(0.35) C42B(0.35)
 C43B(0.35) H43B(0.35) C44B(0.35) H44B(0.35) C45B(0.35) H45B(0.35) C46B(0.35)
 H46B(0.35) C47B(0.35) H47B(0.35) C33A(0.35) C32A(0.35) C36A(0.35) C35A(0.35)
 C34A(0.35) C37A(0.35) H7A(0.35) H7B(0.35) H7C(0.35) C31A(0.35) H8A(0.35)
 H8B(0.35) H8C(0.35) C40A(0.35) H9A(0.35) H9B(0.35) H9C(0.35) C39A(0.35)
 H10A(0.35) H10B(0.35) H10C(0.35) C38A(0.35) H11A(0.35) H11B(0.35) H11C(0.35)
 C36B(0.65) C32B(0.65) C33B(0.65) C34B(0.65) C35B(0.65) C40B(0.65) H40A(0.65)
 H40B(0.65) H40C(0.65) C31B(0.65) H31A(0.65) H31B(0.65) H31C(0.65) C37B(0.65)
 H37A(0.65) H37B(0.65) H37C(0.65) C38B(0.65) H38A(0.65) H38B(0.65) H38C(0.65)
 C39B(0.65) H39A(0.65) H39B(0.65) H39C(0.65) C13A(0.65) H3AA(0.65) H3AB(0.65)
 H3AC(0.65) C15A(0.65) H2AA(0.65) H2AB(0.65) H2AC(0.65) C14A(0.65) H1AA(0.65)
 H1AB(0.65) H1AC(0.65) C15B(0.35) H15A(0.35) H15B(0.35) H15C(0.35) C13B(0.35)
 H13A(0.35) H13B(0.35) H13C(0.35) C14B(0.35) H14A(0.35) H14B(0.35) H14C(0.35)
8.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C3(H3), C21(H21), C4(H4), C22(H22), C19(H19), C5(H5), C20(H20),
 C7(H7), C6(H6), C47A(H13), C46A(H14), C45A(H15), C44A(H16), C43A(H17),
 C43B(H43B), C44B(H44B), C45B(H45B), C46B(H46B), C47B(H47B)
8.b Cp* refined as free rotating group:
 C33A(C32A,C36A,C35A,C34A,C37A,C31A,C40A,C39A,C38A), C36B(C32B,C33B,C34B,C35B,
 C40B,C31B,C37B,C38B,C39B)
8.c Idealised Me refined as rotating group:
 C9(H9D,H9E,H9F), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C25(H25A,H25B,
 H25C), C11(H11D,H11E,H11F), C10(H10D,H10E,H10F), C28(H28A,H28B,H28C), C30(H30A,
 H30B,H30C), C29(H29A,H29B,H29C), C41A(H1A,H1B,H1C), C41B(H41A,H41B,H41C),
 C37A(H7A,H7B,H7C), C31A(H8A,H8B,H8C), C40A(H9A,H9B,H9C), C39A(H10A,H10B,H10C),
 C38A(H11A,H11B,H11C), C40B(H40A,H40B,H40C), C31B(H31A,H31B,H31C), C37B(H37A,
 H37B,H37C), C38B(H38A,H38B,H38C), C39B(H39A,H39B,H39C), C13A(H3AA,H3AB,H3AC),
 C15A(H2AA,H2AB,H2AC), C14A(H1AA,H1AB,H1AC), C15B(H15A,H15B,H15C), C13B(H13A,
 H13B,H13C), C14B(H14A,H14B,H14C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              8340
_shelx_fab_checksum              73123
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'