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_1533009
_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         'C54 H70 Mo2 O4 P4 Sm2, 2(C7 H8)'
_chemical_formula_sum            'C68 H86 Mo2 O4 P4 Sm2'
_chemical_formula_weight         1583.82
_chemical_name_systematic
;
 ?
;
_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             2013-10-17
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2015-05-20 deposited with the CCDC.
2015-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                83.519(6)
_cell_angle_beta                 77.307(6)
_cell_angle_gamma                78.461(6)
_cell_formula_units_Z            1
_cell_length_a                   9.6185(7)
_cell_length_b                   10.2667(7)
_cell_length_c                   17.5096(13)
_cell_measurement_reflns_used    17844
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.71
_cell_measurement_theta_min      2.03
_cell_volume                     1648.4(2)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics
;
Diamond 3,
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
Microsoft Word,
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus100K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      ' 771 frames, detector distance = 60 mm'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1155
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12256
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.246
_diffrn_reflns_theta_min         2.030
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.269
_exptl_absorpt_correction_T_max  0.8387
_exptl_absorpt_correction_T_min  0.5901
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       plate
_exptl_crystal_F_000             794
_exptl_crystal_size_max          0.352
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.071
_refine_diff_density_max         2.832
_refine_diff_density_min         -3.016
_refine_diff_density_rms         0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         5964
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0708
_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^)+(0.1040P)^2^+22.2180P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2034
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4766
_reflns_number_total             5964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02252e2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 1533007--1533012.cif.'
_cod_original_cell_volume        1648.44(21)
_cod_database_code               1533009
_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
Uanis(C22) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C23) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.006 and sigma for
terminal atoms of 0.012
3.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C25(H25), C23(H23), C24(H24), C22(H22), C34(H34), C33(H33),
 C31(H31), C30(H30), C32(H32)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C6(H6A,H6B,H6C),
 C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C),
  C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              15346