The approach to 4d/4f-polyphosphides
Arleth, Nicholas; Gamer, Michael T.; Köppe, Ralf; Pushkarevsky, Nikolay A.; Konchenko, Sergey N.; Fleischmann, Martin; Bodensteiner, Michael; Scheer, Manfred; Roesky, Peter W.; Chem. Sci. 6 (2015) 7179–; doi:10.1039/C5SC02252E

data_1533008
_publ_section_title
;
 The approach to 4d/4f-polyphosphides
;
_journal_issue                   12
_journal_name_full               'Chem. Sci.'
_journal_page_first              7179
_journal_paper_doi               10.1039/C5SC02252E
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C68 H80 Mo4 O8 P2 Yb2'
_chemical_formula_sum            'C68 H80 Mo4 O8 P2 Yb2'
_chemical_formula_weight         1817.10
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-20 deposited with the CCDC.
2015-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                84.903(8)
_cell_angle_beta                 71.669(7)
_cell_angle_gamma                76.285(7)
_cell_formula_units_Z            1
_cell_length_a                   9.4563(7)
_cell_length_b                   12.5189(13)
_cell_length_c                   14.9787(13)
_cell_measurement_reflns_used    11421
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.19
_cell_volume                     1635.0(3)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2009)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED & LANA, PLATON (A.L.Spek, 2009)'
_computing_molecular_graphics    'Diamond 2/3, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'MS Word, Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'two-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5mm monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0761
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14805
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.284
_diffrn_reflns_theta_max         25.284
_diffrn_reflns_theta_min         2.187
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    3.676
_exptl_absorpt_correction_T_max  0.9110
_exptl_absorpt_correction_T_min  0.4969
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_description       needle
_exptl_crystal_F_000             890
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.916
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         5918
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0288P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4341
_reflns_number_total             5918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02252e2.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 1533007--1533012.cif.'
_cod_database_code               1533008
_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. Uiso/Uaniso restraints and constraints
C2A \\sim C3A \\sim C4A \\sim C5A \\sim C7A: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C9B \\sim C10B: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C2A) \\sim Ueq: with sigma of 0.015 and sigma for terminal atoms of 0.02
Uanis(C2B) \\sim Ueq: with sigma of 0.015 and sigma for terminal atoms of 0.02
Uanis(C7B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(C1B)=Sof(C2B)=Sof(C3B)=Sof(C4B)=Sof(C5B)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=
 Sof(H6BC)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(H7BC)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=
 Sof(H8BC)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C10B)=Sof(H10D)=Sof(H10E)=
 Sof(H10F)=1-FVAR(1)
 Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(C4A)=Sof(C5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=
 Sof(H6AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=
 Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C33(H33), C34(H34)
4.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,H7AC), C8A(H8AA,
 H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10A,H10B,H10C), C6B(H6BA,H6BB,H6BC),
 C7B(H7BA,H7BB,H7BC), C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,
 H10F)
;
_shelx_res_checksum              84023
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'