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_1533011
_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 Sm2, 2(C7 H8)'
_chemical_formula_sum            'C78 H106 Mo2 O4 P6 Sm2'
_chemical_formula_weight         1786.02
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-02
_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                98.952(6)
_cell_angle_beta                 110.227(6)
_cell_angle_gamma                95.319(6)
_cell_formula_units_Z            1
_cell_length_a                   11.1671(8)
_cell_length_b                   12.7931(10)
_cell_length_c                   14.7276(9)
_cell_measurement_temperature    123
_cell_volume                     1925.7(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.34a (release 20-07-2010 CrysAlis171 .NET)
(compiled Jul 20 2010,14:26:49)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.34a (release 20-07-2010 CrysAlis171 .NET)
(compiled Jul 20 2010,14:26:49)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.34a (release 20-07-2010 CrysAlis171 .NET)
(compiled Jul 20 2010,14:26:49)
;
_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    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_laue_measured_fraction_full 0.986
_diffrn_reflns_laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15246
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.613
_diffrn_reflns_theta_min         3.264
_exptl_absorpt_coefficient_mu    15.411
_exptl_absorpt_correction_T_max  0.408
_exptl_absorpt_correction_T_min  0.088
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.34a (release 20-07-2010 CrysAlis171 .NET)
(compiled Jul 20 2010,14:26:49)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.4474
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.0955
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         6698
_refine_ls_number_restraints     295
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0419P)^2^+1.0202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6343
_reflns_number_total             6698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02252e2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 1533007--1533012.cif.'
_cod_original_cell_volume        1925.7(2)
_cod_database_code               1533011
_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
 C45-C50 \\sim C49-C50
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C21A \\sim C22A \\sim C23A \\sim C24A \\sim C25A \\sim C26A \\sim C27A \\sim
C28A \\sim C29A \\sim C30A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C21B \\sim C22B \\sim C23B \\sim C24B \\sim C25B \\sim C26B \\sim C27B \\sim
C28B \\sim C29B \\sim C30B: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A: 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: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
C37 \\sim C38 \\sim C39 \\sim C41 \\sim C40 \\sim C42 \\sim C43: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Mo1A) \\sim Ueq, Uanis(Mo2A) \\sim Ueq, Uanis(Mo1B) \\sim Ueq,
Uanis(Mo2B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C50) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: 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) C1B(0.5) C5B(0.5) C4B(0.5) C3B(0.5) C2B(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) 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)
 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) C21A(0.5) C22A(0.5) C23A(0.5)
 C24A(0.5) C25A(0.5) C26A(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C27A(0.5)
 H27A(0.5) H27B(0.5) H27C(0.5) C28A(0.5) H28A(0.5) H28B(0.5) H28C(0.5)
 C29A(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C30A(0.5) H30A(0.5) H30B(0.5)
 H30C(0.5) C21B(0.5) C22B(0.5) C23B(0.5) C24B(0.5) C25B(0.5) C26B(0.5)
 H26D(0.5) H26E(0.5) H26F(0.5) C27B(0.5) H27D(0.5) H27E(0.5) H27F(0.5)
 C28B(0.5) H28D(0.5) H28E(0.5) H28F(0.5) C29B(0.5) H29D(0.5) H29E(0.5)
 H29F(0.5) C30B(0.5) H30D(0.5) H30E(0.5) H30F(0.5) P1(0.5) P2(0.5) P3(0.5)
 P4(0.5) P5(0.5) P6(0.5) Mo2B(0.25) C31(0.5) O1(0.5) C33(0.25) O3(0.25)
 C34(0.25) O4(0.25) C32(0.5) O2(0.5) C35(0.25) O5(0.25) C36(0.25) O6(0.25)
 C37(0.62) C38(0.62) H38(0.62) C39(0.62) H39(0.62) C40(0.62) H40(0.62)
 C41(0.62) H41(0.62) C42(0.62) H42(0.62) C43(0.62) H43A(0.62) H43B(0.62)
 H43C(0.62) C44(0.38) C45(0.38) H45(0.38) C46(0.38) H46(0.38) C47(0.38)
 H47(0.38) C48(0.38) H48(0.38) C49(0.38) H49(0.38) C50(0.38) H50A(0.38)
 H50B(0.38) H50C(0.38) Mo1B(0.25) Mo1A(0.25) Mo2A(0.25)
5.a Me refined with riding coordinates:
 C50(H50A,H50B,H50C)
5.b Aromatic/amide H refined with riding coordinates:
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C45(H45), C46(H46),
 C47(H47), C48(H48), C49(H49)
5.c Fitted pentagon refined as free rotating group:
 C1B(C5B,C4B,C3B,C2B)
5.d Fitted hexagon refined as free rotating group:
 C37(C38,C39,C40,C41,C42), C44(C45,C46,C47,C48,C49)
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), C6B(H6BA,H6BB,H6BC), C7B(H7BA,H7BB,H7BC),
 C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F), 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), C26A(H26A,H26B,H26C),
 C27A(H27A,H27B,H27C), C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C), C30A(H30A,
 H30B,H30C), C26B(H26D,H26E,H26F), C27B(H27D,H27E,H27F), C28B(H28D,H28E,H28F),
 C29B(H29D,H29E,H29F), C30B(H30D,H30E,H30F), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              67357
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'