(Ge<sub>2</sub>P<sub>2</sub>)<sup>2-</sup>: a binary analogue of P<sub>4</sub> as a precursor to the ternary cluster anion [Cd<sub>3</sub>(Ge<sub>3</sub>P)<sub>3</sub>]<sup>3</sup>.
Mitzinger, Stefan; Bandemehr, Jascha; Reiter, Kevin; Scott McIndoe, J.; Xie, Xiulan; Weigend, Florian; Corrigan, John F.; Dehnen, Stefanie; Chemical communications (Cambridge, England) 54 (2018) 1421–1424; doi:10.1039/c7cc08348c

data_7121041
_publ_section_title
;
 (Ge<sub>2</sub>P<sub>2</sub>)<sup>2-</sup>: a binary analogue of
 P<sub>4</sub> as a precursor to the ternary cluster anion
 [Cd<sub>3</sub>(Ge<sub>3</sub>P)<sub>3</sub>]<sup>3</sup>.
;
_journal_issue                   12
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1421
_journal_page_last               1424
_journal_paper_doi               10.1039/c7cc08348c
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety
'2(C18 H36 K N2 O6), 0.17(C150 H264 K6 N12 O36), 0.5(Cd6 Ge18 P6)'
_chemical_formula_sum            'C61 H116 Cd3 Ge9 K3 N6 O18 P3'
_chemical_formula_weight         2422.52
_space_group_crystal_system      hexagonal
_space_group_IT_number           179
_space_group_name_Hall           'P 65 2 (0 0 1)'
_space_group_name_H-M_alt        'P 65 2 2'
_symmetry_space_group_name_Hall  'P 65 2 (0 0 1)'
_symmetry_space_group_name_H-M   'P 65 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-10-12
_audit_creation_method
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-13 deposited with the CCDC.
2017-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.237(2)
_cell_length_b                   15.237(2)
_cell_length_c                   68.672(14)
_cell_measurement_reflns_used    132693
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.660
_cell_measurement_theta_min      2.356
_cell_volume                     13807(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Quest'
_diffrn_measurement_method       'CCD Detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       83
_diffrn_reflns_limit_l_min       -83
_diffrn_reflns_number            132693
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.660
_diffrn_reflns_theta_max         25.660
_diffrn_reflns_theta_min         2.356
_exptl_absorpt_coefficient_mu    3.816
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       block
_exptl_crystal_F_000             7211
_refine_diff_density_max         1.203
_refine_diff_density_min         -1.233
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.10(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         8698
_refine_ls_number_restraints     313
_refine_ls_restrained_S_all      1.416
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0733
_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^)+(0.0633P)^2^+128.8772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1743
_refine_ls_wR_factor_ref         0.1796
_reflns_Friedel_coverage         0.680
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7688
_reflns_number_total             8698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc08348c2.cif
_cod_data_source_block           jb94_0m_pl
_cod_depositor_comments
'Adding full bibliography for 7121039--7121041.cif.'
_cod_original_cell_volume        13807(5)
_cod_database_code               7121041
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.90(4)
 0.10(4)
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. Restrained distances
 C4A-C3A
 1.49 with sigma of 0.02
 C15A-C16A
 1.49 with sigma of 0.02
 C17A-C18A
 1.49 with sigma of 0.02
 C16A-C15A
 1.49 with sigma of 0.02
 C14A-C13A
 1.49 with sigma of 0.02
 C1A-C2A
 1.49 with sigma of 0.02
 C3A-C4A
 1.49 with sigma of 0.02
 C5A-C6A
 1.49 with sigma of 0.02
 C12A-C11A
 1.49 with sigma of 0.02
 C10A-C9A
 1.49 with sigma of 0.02
 C8A-C7A
 1.49 with sigma of 0.02
 C5B-C6B
 1.49 with sigma of 0.02
 C6B-C5B
 1.49 with sigma of 0.02
 C4B-C3B
 1.49 with sigma of 0.02
 C2B-C1B
 1.49 with sigma of 0.02
 C9B-C9B
 1.49 with sigma of 0.02
 C8B-C7B
 1.49 with sigma of 0.02
 C20-C21
 1.4 with sigma of 0.02
 C22-C21
 1.4 with sigma of 0.02
 C22-C23
 1.4 with sigma of 0.02
4. Restrained planarity
 C20, C21, C22, C23
 with sigma of 0.1
5. Rigid bond restraints
 C19, C20, C21, C22, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6. Uiso/Uaniso restraints and constraints
C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C7B) = Uanis(C9B)
Uanis(C1B) = Uanis(C7B)
Uanis(C2B) = Uanis(C8B)
Uanis(C3B) = Uanis(C9B)
Uanis(O1A) = Uanis(O3A)
Uanis(O2A) = Uanis(O4A)
Uanis(O2B) = Uanis(O3B)
Uanis(C23) = Uanis(C19)
7. Rigid body (RIGU) restrains
 C19, C20, C21, C22, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1B, O2B, O3B, N1B, C1B, C9B, C2B, C3B, C4B, C5B, C6B, C7B, C8B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1A, O2A, O3A, O4A, O5A, O6A, N1A, N2A, C10A, C1A, C2A, C3A, C4A, C5A, C6A,
 C7A, C8A, C9A, C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
8. Same fragment restrains
{C19, C20, C21, C22, C23} sigma for 1-2: 0.02, 1-3: 0.04
as
{O1A, O2A, O3A, O4A, O5A}
9. Others
 Fixed Sof: Cd2A(0.5) Cd2B(0.5) Ge1(0.5) Ge2(0.5) Ge3(0.5) Ge4(0.5) Ge5(0.5)
 Ge6(0.5) P1(0.5) P3(0.5) Ge7(0.5) Ge8(0.5) P2(0.5) H19A(0.5) H19B(0.5)
 H19C(0.5) Ge9(0.5) Cd0A(0.5)
10.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C2A(H2AA,H2AB), C3A(H3AA,H3AB), C4A(H4AA,H4AB), C5A(H5AA,
 H5AB), C6A(H6AA,H6AB), C7A(H7AA,H7AB), C8A(H8AA,H8AB), C9A(H9AA,H9AB),
 C10A(H10A,H10B), C11A(H11A,H11B), C12A(H12A,H12B), C13A(H13A,H13B), C14A(H14A,
 H14B), C15A(H15A,H15B), C16A(H16A,H16B), C17A(H17A,H17B), C18A(H18A,H18B),
 C1B(H1BA,H1BB), C2B(H2BA,H2BB), C3B(H3BA,H3BB), C4B(H4BA,H4BB), C5B(H5BA,H5BB),
  C6B(H6BA,H6BB), C7B(H7BA,H7BB), C8B(H8BA,H8BB), C9B(H9BA,H9BB)
10.b Me refined with riding coordinates:
 C19(H19A,H19B,H19C)
10.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C23(H23)
;
_shelx_res_checksum              2313
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
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;