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_7127009
_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, 2(C7 H8)'
_chemical_formula_sum            'C54 H77 Fe Ge2 N4 P5'
_chemical_formula_weight         1138.07
_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             2020-03-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-03 deposited with the CCDC.	2020-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                84.679(10)
_cell_angle_beta                 79.665(7)
_cell_angle_gamma                83.291(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1225(10)
_cell_length_b                   14.174(2)
_cell_length_c                   16.7654(17)
_cell_measurement_reflns_used    18626
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      1.72
_cell_volume                     2807.0(5)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (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      150.0
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
 190 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28119
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.504
_diffrn_reflns_theta_min         1.717
_exptl_absorpt_coefficient_mu    1.500
_exptl_absorpt_correction_T_max  0.8851
_exptl_absorpt_correction_T_min  0.5593
_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 brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.073
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         15293
_refine_ls_number_restraints     468
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0386P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9972
_reflns_number_total             15293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03920a2.cif
_cod_data_source_block           ry452
_cod_depositor_comments
'Adding full bibliography for 7127008--7127009.cif.'
_cod_original_cell_volume        2807.1(6)
_cod_database_code               7127009
_shelx_shelxl_version_number     2018/3
_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
 C42B-C43B \\sim C43B-C44B \\sim C44B-C45B \\sim C45B-C46B \\sim C46B-C47B
\\sim C47B-C42B
 with sigma of 0.02
 C42B-C46B \\sim C42B-C44B \\sim C47B-C45B \\sim C43B-C47B \\sim C44B-C46B
\\sim C43B-C45B
 with sigma of 0.04
 C41B-C47B \\sim C41B-C43B
 with sigma of 0.04
 C49B-C50B \\sim C50B-C51B \\sim C51B-C52B \\sim C52B-C53B \\sim C53B-C54B
\\sim C54B-C49B
 with sigma of 0.02
 C49B-C53B \\sim C49B-C51B \\sim C54B-C52B \\sim C50B-C54B \\sim C51B-C53B
\\sim C50B-C52B
 with sigma of 0.04
 C48A-C54B \\sim C48A-C50B
 with sigma of 0.04
 C42A-C43A \\sim C43A-C44A \\sim C44A-C45A \\sim C45A-C46A \\sim C46A-C47A
\\sim C47A-C42A
 with sigma of 0.02
 C42A-C46A \\sim C42A-C44A \\sim C47A-C45A \\sim C43A-C47A \\sim C44A-C46A
\\sim C43A-C45A
 with sigma of 0.04
 C41A-C47A \\sim C41A-C43A
 with sigma of 0.04
 C49A-C50A \\sim C50A-C51A \\sim C51A-C52A \\sim C52A-C53A \\sim C53A-C54A
\\sim C54A-C49A
 with sigma of 0.02
 C49A-C53A \\sim C49A-C51A \\sim C54A-C52A \\sim C50A-C54A \\sim C51A-C53A
\\sim C50A-C52A
 with sigma of 0.04
 C48B-C54A \\sim C48B-C50A
 with sigma of 0.04
3. Restrained planarity
 C41B, C42B, C43B, C44B, C45B, C46B, C47B
 with sigma of 0.1
 C48A, C49B, C50B, C51B, C52B, C53B, C54B
 with sigma of 0.1
 C41A, C42A, C43A, C44A, C45A, C46A, C47A
 with sigma of 0.1
 C48B, C49A, C50A, C51A, C52A, C53A, C54A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
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
C48A \\sim C49B \\sim C50B \\sim C51B \\sim C52B \\sim C53B \\sim C54B: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C41A \\sim C42A \\sim C43A \\sim C44A \\sim C45A \\sim C46A \\sim C47A: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C48B \\sim C49A \\sim C50A \\sim C51A \\sim C52A \\sim C53A \\sim C54A: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 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
 C48A, C49B, C50B, C51B, C52B, C53B, C54B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41A, C42A, C43A, C44A, C45A, C46A, C47A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C48B, C49A, C50A, C51A, C52A, C53A, C54A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C48A(0.5) H48D(0.5) H48E(0.5) H48F(0.5) C48B(0.5) H48A(0.5)
 H48B(0.5) H48C(0.5) C49A(0.5) C49B(0.5) C50A(0.5) H50A(0.5) C50B(0.5)
 H50B(0.5) C51A(0.5) H51A(0.5) C51B(0.5) H51B(0.5) C52A(0.5) H52A(0.5)
 C52B(0.5) H52B(0.5) C53A(0.5) H53A(0.5) C53B(0.5) H53B(0.5) C54A(0.5)
 H54A(0.5) C54B(0.5) H54B(0.5) C41A(0.5) H41D(0.5) H41E(0.5) H41F(0.5)
 C41B(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C42A(0.5) C42B(0.5) C43A(0.5)
 H43A(0.5) C43B(0.5) H43B(0.5) C44A(0.5) H44A(0.5) C44B(0.5) H44B(0.5)
 C45A(0.5) H45A(0.5) C45B(0.5) H45B(0.5) C46A(0.5) H46A(0.5) C46B(0.5)
 H46B(0.5) C47A(0.5) H47A(0.5) C47B(0.5) H47B(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C28(H28), C29(H29),
 C30(H30), C31(H31), C32(H32), C50A(H50A), C50B(H50B), C51A(H51A), C51B(H51B),
 C52A(H52A), C52B(H52B), C53A(H53A), C53B(H53B), C54A(H54A), C54B(H54B),
 C43A(H43A), C43B(H43B), C44A(H44A), C44B(H44B), C45A(H45A), C45B(H45B),
 C46A(H46A), C46B(H46B), C47A(H47A), C47B(H47B)
7.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C), C48A(H48D,H48E,H48F), C48B(H48A,H48B,H48C),
 C41A(H41D,H41E,H41F), C41B(H41A,H41B,H41C)
;
_shelx_res_checksum              91067
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'