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_1533007
_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 Sm2, C7 H8'
_chemical_formula_sum            'C75 H88 Mo4 O8 P2 Sm2'
_chemical_formula_weight         1863.85
_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                97.784(3)
_cell_angle_beta                 90.790(3)
_cell_angle_gamma                100.069(3)
_cell_formula_units_Z            1
_cell_length_a                   9.5023(3)
_cell_length_b                   12.6103(4)
_cell_length_c                   15.1418(5)
_cell_measurement_reflns_used    16204
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.77
_cell_measurement_theta_min      1.36
_cell_volume                     1768.68(10)
_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 0.997
_diffrn_measured_fraction_theta_max 0.991
_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  0.0684
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17149
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.100
_diffrn_reflns_theta_min         1.358
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_type              'Xenocs Genix3D microfocus'
_exptl_absorpt_coefficient_mu    2.420
_exptl_absorpt_correction_T_max  0.6677
_exptl_absorpt_correction_T_min  0.1479
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED, X-SHAPE & LANA'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_description       needle
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.043
_refine_diff_density_max         3.111
_refine_diff_density_min         -2.070
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         6969
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0912P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1389
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5361
_reflns_number_total             6969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc02252e2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 1533007--1533012.cif.'
_cod_database_code               1533007
_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
C35 \\sim C36 \\sim C41 \\sim C40 \\sim C39 \\sim C38 \\sim C37: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C36(0.5) C37(0.5) H37(0.5)
 C38(0.5) H38(0.5) C39(0.5) H39(0.5) C40(0.5) H40(0.5) C41(0.5) H41(0.5)
4.a Free rotating group:
 C35(C36,C37,C38,C39,C40,C41)
4.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C30(H30), C31(H31), C32(H32), C33(H33), C28(H28), C27(H27),
 C26(H26), C25(H25), C29(H29), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
4.c 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), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C6(H6A,H6B,H6C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              89842
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'