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_7037610
_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         'C48 H88 N8 Na4'
_chemical_formula_sum            'C48 H88 N8 Na4'
_chemical_formula_weight         869.22
_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/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-09-09
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-10-24 deposited with the CCDC.
2015-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.129(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.1838(8)
_cell_length_b                   10.7957(5)
_cell_length_c                   17.0882(9)
_cell_measurement_reflns_used    7141
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      29.5538
_cell_measurement_theta_min      3.3066
_cell_volume                     2690.8(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
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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)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      123.1
_diffrn_detector_area_resol_mean 16.0727
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details
;
  1 omega   37.00   87.00   1.0000   54.8500
omega____ theta____ kappa____ phi______ frames
    -       19.4192  179.0000    0.0000 50

  2 omega  -39.00   75.00   1.0000   54.8500
omega____ theta____ kappa____ phi______ frames
    -       19.4192    0.0000  -90.0000 114

  3 omega  -89.00  -42.00   1.0000   54.8500
omega____ theta____ kappa____ phi______ frames
    -      -20.2005  154.0000 -114.0000 47

  4 omega  -11.00   90.00   1.0000   54.8500
omega____ theta____ kappa____ phi______ frames
    -       19.4192   77.0000   60.0000 101

  5 omega   -6.00   92.00   1.0000   54.8500
omega____ theta____ kappa____ phi______ frames
    -       19.4192   37.0000  -30.0000 98

  6 omega  -95.00  -40.00   1.0000   54.8500
omega____ theta____ kappa____ phi______ frames
    -      -20.2005  154.0000   65.0000 55
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0220691000
_diffrn_orient_matrix_UB_12      0.0433423000
_diffrn_orient_matrix_UB_13      -0.0303244000
_diffrn_orient_matrix_UB_21      -0.0040362000
_diffrn_orient_matrix_UB_22      -0.0460786000
_diffrn_orient_matrix_UB_23      -0.0303497000
_diffrn_orient_matrix_UB_31      -0.0431228000
_diffrn_orient_matrix_UB_32      -0.0178802000
_diffrn_orient_matrix_UB_33      0.0049085000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26046
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.997
_diffrn_reflns_theta_min         3.313
_diffrn_source                   'Oxford Diffraction Xcalibur E'
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.073
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         6829
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0690P)^2^+1.1215P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1521
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4827
_reflns_number_total             6829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04224k2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7037610--7037614.cif.'
_cod_database_code               7037610
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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. Restrained distances
 C1A-C2A
 1.39 with sigma of 0.01
 C3A-C2A
 1.44 with sigma of 0.01
 C3A-C4A
 1.34 with sigma of 0.01
 C4A-C5A
 1.5 with sigma of 0.01
 C5A-C6A = C6A-C7A = C6A-C8A = C6A-C9A
 1.535 with sigma of 0.01
 N1A-C1A
 1.33 with sigma of 0.01
 N1A-C5A
 1.48 with sigma of 0.01
 C5A-C7A = C5A-C9A = C5A-C8A
 2.5 with sigma of 0.01
 C1A-C5A
 2.3 with sigma of 0.01
 C7A-C8A = C8A-C9A = C9A-C7A
 2.47 with sigma of 0.01
3. Rigid bond restraints
 N1, C1, C2, C3, C4, C5, C6, C7, C8, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8
\\sim C9: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(N1) = Uanis(N1A)
Uanis(C1) = Uanis(C1A)
Uanis(C2) = Uanis(C2A)
Uanis(C3) = Uanis(C3A)
Uanis(C4) = Uanis(C4A)
Uanis(C5) = Uanis(C5A)
Uanis(C6) = Uanis(C6A)
Uanis(C7) = Uanis(C7A)
Uanis(C8) = Uanis(C8A)
Uanis(C9) = Uanis(C9A)
5. Others
 Sof(N1A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=
 Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(C7A)=Sof(H7A1)=Sof(H7A2)=Sof(H7A3)=
 Sof(C8A)=Sof(H8A1)=Sof(H8A2)=Sof(H8A3)=Sof(C9A)=Sof(H9A1)=Sof(H9A2)=Sof(H9A3)=
 1-FVAR(1)
 Sof(N1)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=
 Sof(C5)=Sof(H5)=Sof(C6)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=
 Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C5(H5), C14(H14), C5A(H5A)
6.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B)
6.c Me refined with riding coordinates:
 C7A(H7A1,H7A2,H7A3), C8A(H8A1,H8A2,H8A3), C9A(H9A1,H9A2,H9A3)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C10(H10), C11(H11), C12(H12), C13(H13),
 C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A)
6.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_olex2_submission_original_sample_id RMSO4
_olex2_submission_special_instructions 'No special instructions were received'