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_1533010
_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         'C81 H105 Mo3 O6 P5 Sm3'
_chemical_formula_sum            'C81 H105 Mo3 O6 P5 Sm3'
_chemical_formula_weight         2068.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-07
_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                90
_cell_angle_beta                 96.36(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.130(2)
_cell_length_b                   25.686(5)
_cell_length_c                   15.724(3)
_cell_measurement_temperature    100
_cell_volume                     4066.2(14)
_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 1.000
_diffrn_measured_fraction_theta_max 0.986
_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  0.2911
_diffrn_reflns_av_unetI/netI     0.1896
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33852
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.198
_diffrn_reflns_theta_min         1.303
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_type              'Xenocs Genix3D microfocus'
_exptl_absorpt_coefficient_mu    2.727
_exptl_absorpt_correction_T_max  0.9407
_exptl_absorpt_correction_T_min  0.8569
_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    1.689
_exptl_crystal_description       block
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.069
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.051
_refine_diff_density_max         3.711
_refine_diff_density_min         -2.082
_refine_diff_density_rms         0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         7394
_refine_ls_number_restraints     398
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.1889
_refine_ls_R_factor_gt           0.1092
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1535P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2500
_refine_ls_wR_factor_ref         0.2946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3627
_reflns_number_total             7394
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02252e2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1533007--1533012.cif.'
_cod_original_cell_volume        4066.3(14)
_cod_database_code               1533010
_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
 C13B-C19B
 2.6 with sigma of 0.02
 C15B-C19B
 2.6 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim
C9A \\sim C10A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim C7B \\sim C8B \\sim
C9B \\sim C10B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C11A \\sim C12A \\sim C13A \\sim C14A \\sim C15A \\sim C16A \\sim C17A \\sim
C18A \\sim C19A \\sim C20A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C11B \\sim C12B \\sim C13B \\sim C14B \\sim C15B \\sim C16B \\sim C17B \\sim
C18B \\sim C19B \\sim C20B: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C25 \\sim C29 \\sim C28 \\sim C27 \\sim C26: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim
C40 \\sim C41: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C44 \\sim C43 \\sim C42 \\sim C47 \\sim C46 \\sim C45: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6A) \\sim Ueq, Uanis(C9B) \\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C19B)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C30B) = Uanis(C30A)
4. Others
 Fixed Sof: P1(0.5) P2(0.5) P3(0.5) P4(0.5) P5(0.5) O1A(0.5) O1B(0.5) O2B(0.5)
 O2A(0.5) H45A(0.5) H45B(0.5) H45C(0.5) C5A(0.5) C1A(0.5) C2A(0.5) C3A(0.5)
 C4A(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) C12A(0.5) C13A(0.5)
 C14A(0.5) C15A(0.5) C11A(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) 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) C5B(0.5) C1B(0.5)
 C2B(0.5) C3B(0.5) C4B(0.5) C10B(0.5) H10D(0.5) H10E(0.5) H10F(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) C30B(0.5)
 C30A(0.5) C33(0.5) C34(0.5) C35(0.5) C36(0.5) C32(0.5) C38(0.5) H38A(0.5)
 H38B(0.5) H38C(0.5) C39(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C40(0.5) H40A(0.5)
 H40B(0.5) H40C(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C37(0.5) H37A(0.5)
 H37B(0.5) H37C(0.5)
5.a Ternary CH refined with riding coordinates:
 C22(H22), C23(H23), C24(H24)
5.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29)
5.c Fitted pentagon refined as free rotating group:
 C5A(C1A,C2A,C3A,C4A), C12A(C13A,C14A,C15A,C11A), C11B(C12B,C13B,C14B,C15B),
 C5B(C1B,C2B,C3B,C4B)
5.d Cp* refined as free rotating group:
 C33(C34,C35,C36,C32,C38,C39,C40,C41,C37)
5.e Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), 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), C16B(H16D,H16E,H16F),
 C17B(H17D,H17E,H17F), C18B(H18D,H18E,H18F), C19B(H19D,H19E,H19F), C20B(H20D,
 H20E,H20F), C10B(H10D,H10E,H10F), C6B(H6BA,H6BB,H6BC), C7B(H7BA,H7BB,H7BC),
 C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              87087
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'