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_7037612
_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         'C30 H60 K2 N6'
_chemical_formula_sum            'C30 H60 K2 N6'
_chemical_formula_weight         583.04
_chemical_name_systematic        RMSO5
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-17
_audit_creation_method
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Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-10-24 deposited with the CCDC.
2015-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.489(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6958(10)
_cell_length_b                   8.9464(5)
_cell_length_c                   18.0264(9)
_cell_measurement_reflns_used    5103
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      29.4527
_cell_measurement_theta_min      3.2822
_cell_volume                     3649.0(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_details
;
  1 omega    9.00   92.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4192   37.0000 -150.0000 83

  2 omega   -5.00   90.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4192   77.0000  -90.0000 95

  3 omega  -72.00  -22.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2005  118.0000  -45.0000 50

  4 omega   -6.00   92.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4192   37.0000  120.0000 98

  5 omega   34.00   82.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4192  179.0000  150.0000 48

  6 omega  -51.00   49.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       19.4192  -77.0000 -180.0000 100
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0104744000
_diffrn_orient_matrix_UB_12      0.0073089000
_diffrn_orient_matrix_UB_13      -0.0380084000
_diffrn_orient_matrix_UB_21      -0.0284829000
_diffrn_orient_matrix_UB_22      0.0183620000
_diffrn_orient_matrix_UB_23      0.0108674000
_diffrn_orient_matrix_UB_31      0.0077854000
_diffrn_orient_matrix_UB_32      0.0766607000
_diffrn_orient_matrix_UB_33      0.0009503000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18020
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         3.289
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4611
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+3.2419P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3325
_reflns_number_total             4611
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04224k2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7037610--7037614.cif.'
_cod_database_code               7037612
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.60
_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
 C6-C7 = C6-C8 = C6-C9 = C21-C22 = C21-C23 = C21-C24
 1.53 with sigma of 0.01
 N4-C16
 1.34 with sigma of 0.01
 N4-C20
 1.48 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
 N4, C16, C17, C18, C19, C20, C21, C22, C23, C24
 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
N4 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim
C23 \\sim C24: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
Uanis(C1) = Uanis(C16)
Uanis(C6) = Uanis(C21)
Uanis(N1) = Uanis(N4)
Uanis(C2) = Uanis(C17)
5. Others
 Sof(N4)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=
 Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 1-FVAR(1)
 Sof(N1)=Sof(C1)=Sof(H7)=Sof(C2)=Sof(H8)=Sof(C3)=Sof(H9)=Sof(C4)=Sof(H10)=
 Sof(C5)=Sof(H11)=Sof(C6)=Sof(C7)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C8)=
 Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C9)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C5(H11), C18(H18), C19(H19), C20(H20)
6.b Secondary CH2 refined with riding coordinates:
 C12(H3A,H3B), C13(H4A,H4B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H7), C2(H8), C3(H9), C4(H10), C16(H16), C17(H17)
6.d Idealised Me refined as rotating group:
 C10(H1A,H1B,H1C), C7(H13A,H13B,H13C), C8(H14A,H14B,H14C), C9(H15A,H15B,H15C),
 C11(H2A,H2B,H2C), C14(H5A,H5B,H5C), C15(H6A,H6B,H6C), C22(H22A,H22B,H22C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_olex2_submission_original_sample_id RMSO5
_olex2_submission_special_instructions 'No special instructions were received'