Accessible heavier s-block dihydropyridines: structural elucidation and reactivity of isolable molecular hydride sources.
Orr, Samantha A.; Kennedy, Alan R.; Liggat, John J.; McLellan, Ross; Mulvey, Robert E.; Robertson, Stuart D.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 6234–6240; doi:10.1039/c5dt04224k

data_7037611
_publ_section_title
;
 Accessible heavier s-block dihydropyridines: structural elucidation and
 reactivity of isolable molecular hydride sources.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6234
_journal_page_last               6240
_journal_paper_doi               10.1039/c5dt04224k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C36 H74 N8 Na2'
_chemical_formula_sum            'C36 H74 N8 Na2'
_chemical_formula_weight         665.02
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
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Olex2 1.2
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_audit_update_record
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2015-10-24 deposited with the CCDC.
2015-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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  1 omega -100.00   16.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.5801  -37.0000  170.0000 116

  2 omega  -96.00   18.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.5801  -37.0000  -60.0000 114

  3 omega -109.00  -32.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.5801  179.0000    0.0000 77

  4 omega  -98.00  -73.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.5801  -77.0000   90.0000 25

  5 omega  -64.00   55.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.5801   37.0000  -30.0000 119
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_diffrn_orient_matrix_UB_32      0.0163750000
_diffrn_orient_matrix_UB_33      -0.0350252000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_unetI/netI     0.0438
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_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         26.98
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_diffrn_source                   'Oxford Diffraction Xcalibur E'
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  1.00000
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
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_exptl_crystal_density_diffrn    1.0474
_exptl_crystal_description       fragment
_exptl_crystal_F_000             736.3194
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_exptl_crystal_size_mid          0.2
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_refine_ls_restrained_S_all      1.0471
_refine_ls_R_factor_all          0.0863
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+1.0361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_limit_l_min              -8
_reflns_number_gt                3204
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_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt04224k2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7037610--7037614.cif.'
_cod_database_code               7037611
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12b,H12a), C13(H13a,H13b), C15(H15a,H15b), C16(H16a,H16b)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5)
2.d Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C10(H10c,H10a,H10b),
 C11(H11a,H11b,H11c), C14(H14a,H14b,H14c), C17(H17a,H17b,H17c), C18(H18a,H18b,
 H18c)
;
_olex2_submission_original_sample_id RMSO3
_olex2_submission_special_instructions 'No special instructions were received'