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_1533012
_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         'C64 H90 Mo2 O4 P6 Yb2, 2(C7 H8)'
_chemical_formula_sum            'C78 H106 Mo2 O4 P6 Yb2'
_chemical_formula_weight         1831.40
_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             2015-03-30
_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                99.581(2)
_cell_angle_beta                 110.455(2)
_cell_angle_gamma                94.847(2)
_cell_formula_units_Z            1
_cell_length_a                   11.1924(3)
_cell_length_b                   12.6285(3)
_cell_length_c                   14.6371(4)
_cell_measurement_reflns_used    31280
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.06
_cell_measurement_theta_min      1.97
_cell_volume                     1888.44(9)
_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      100
_diffrn_detector                 'CMOS pixel detector'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 100k'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'single reflection optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_laue_measured_fraction_full 0.987
_diffrn_reflns_laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17122
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.042
_diffrn_reflns_theta_min         1.966
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_type              'Xenocs Genix3D microfocus'
_exptl_absorpt_coefficient_mu    2.952
_exptl_absorpt_correction_T_max  0.8814
_exptl_absorpt_correction_T_min  0.6591
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED, X-SHAPE & LANA'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.049
_refine_diff_density_max         2.964
_refine_diff_density_min         -2.488
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         7340
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0433P)^2^+10.1569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1033
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6799
_reflns_number_total             7340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02252e2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 1533007--1533012.cif.'
_cod_database_code               1533012
_shelxl_version_number           2014/7
_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
 C42-C40
 2.5 with sigma of 0.005
 C46-C40
 2.5 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C1B) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C14A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: P1(0.5) P2(0.5) P3(0.5) P4(0.5) P5(0.5) P6(0.5) O1A(0.5) O2A(0.25)
 O2C(0.25) O1B(0.5) O2B(0.25) O2D(0.25) C1A(0.5) C2A(0.5) C3A(0.5) C4A(0.5)
 C5A(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5) H6AC(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5)
 H7AC(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5) H8AC(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5)
 H9AC(0.5) C10A(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C11A(0.5) C12A(0.5)
 C13A(0.5) C14A(0.5) C15A(0.5) C16A(0.5) H16A(0.5) H16B(0.5) H16C(0.5)
 C17A(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C18A(0.5) H18A(0.5) H18B(0.5)
 H18C(0.5) C19A(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C20A(0.5) H20A(0.5)
 H20B(0.5) H20C(0.5) C21A(0.34) C22A(0.34) C23A(0.34) C24A(0.34) C25A(0.34)
 C26A(0.34) H26A(0.34) H26B(0.34) H26C(0.34) C27A(0.34) H27A(0.34) H27B(0.34)
 H27C(0.34) C28A(0.34) H28A(0.34) H28B(0.34) H28C(0.34) C29A(0.34) H29A(0.34)
 H29B(0.34) H29C(0.34) C30A(0.34) H30A(0.34) H30B(0.34) H30C(0.34) C31A(0.5)
 C32A(0.25) C32C(0.25) C1B(0.5) C2B(0.5) C3B(0.5) C4B(0.5) C5B(0.5) C6B(0.5)
 H6BA(0.5) H6BB(0.5) H6BC(0.5) C7B(0.5) H7BA(0.5) H7BB(0.5) H7BC(0.5) C8B(0.5)
 H8BA(0.5) H8BB(0.5) H8BC(0.5) C9B(0.5) H9BA(0.5) H9BB(0.5) H9BC(0.5) C10B(0.5)
 H10D(0.5) H10E(0.5) H10F(0.5) C11B(0.5) C12B(0.5) C13B(0.5) C14B(0.5)
 C15B(0.5) C16B(0.5) H16D(0.5) H16E(0.5) H16F(0.5) C17B(0.5) H17D(0.5)
 H17E(0.5) H17F(0.5) C18B(0.5) H18D(0.5) H18E(0.5) H18F(0.5) C19B(0.5)
 H19D(0.5) H19E(0.5) H19F(0.5) C20B(0.5) H20D(0.5) H20E(0.5) H20F(0.5)
 C21B(0.33) C22B(0.33) C23B(0.33) C24B(0.33) C25B(0.33) C26B(0.33) H26D(0.33)
 H26E(0.33) H26F(0.33) C27B(0.33) H27D(0.33) H27E(0.33) H27F(0.33) C28B(0.33)
 H28D(0.33) H28E(0.33) H28F(0.33) C29B(0.33) H29D(0.33) H29E(0.33) H29F(0.33)
 C30B(0.33) H30D(0.33) H30E(0.33) H30F(0.33) C31B(0.5) C32B(0.25) C32D(0.25)
 C21C(0.33) C22C(0.33) C23C(0.33) C24C(0.33) C25C(0.33) C26C(0.33) H26G(0.33)
 H26H(0.33) H26I(0.33) C27C(0.33) H27G(0.33) H27H(0.33) H27I(0.33) C28C(0.33)
 H28G(0.33) H28H(0.33) H28I(0.33) C29C(0.33) H29G(0.33) H29H(0.33) H29I(0.33)
 C30C(0.33) H30G(0.33) H30H(0.33) H30I(0.33) C40(0.5) H40A(0.5) H40B(0.5)
 H40C(0.5) C41(0.5) C42(0.5) H42(0.5) C43(0.5) H43(0.5) C44(0.5) H44(0.5)
 C45(0.5) H45(0.5) C46(0.5) H46(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5)
 C34(0.5) C35(0.5) H35(0.5) C36(0.5) H36(0.5) C37(0.5) H37(0.5) C38(0.5)
 H38(0.5) C39(0.5) H39(0.5)
5.a :
 C11B(C12B,C13B,C14B,C15B)
5.b Me refined with riding coordinates:
 C40(H40A,H40B,H40C)
5.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C35(H35), C36(H36),
 C37(H37), C38(H38), C39(H39)
5.d Fitted hexagon refined as free rotating group:
 C41(C42,C43,C44,C45,C46), C34(C35,C36,C37,C38,C39)
5.e Idealised Me refined as rotating group:
 C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,
 H9AC), C10A(H10A,H10B,H10C), C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C),
 C18A(H18A,H18B,H18C), C19A(H19A,H19B,H19C), C20A(H20A,H20B,H20C), C26A(H26A,
 H26B,H26C), C27A(H27A,H27B,H27C), C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C),
 C30A(H30A,H30B,H30C), C6B(H6BA,H6BB,H6BC), C7B(H7BA,H7BB,H7BC), C8B(H8BA,H8BB,
 H8BC), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F), C16B(H16D,H16E,H16F),
 C17B(H17D,H17E,H17F), C18B(H18D,H18E,H18F), C19B(H19D,H19E,H19F), C20B(H20D,
 H20E,H20F), C26B(H26D,H26E,H26F), C27B(H27D,H27E,H27F), C28B(H28D,H28E,H28F),
 C29B(H29D,H29E,H29F), C30B(H30D,H30E,H30F), C26C(H26G,H26H,H26I), C27C(H27G,
 H27H,H27I), C28C(H28G,H28H,H28I), C29C(H29G,H29H,H29I), C30C(H30G,H30H,H30I),
 C33(H33A,H33B,H33C)
;
_shelx_res_checksum              17414
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'