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_7037614
_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         'C26 H44 K2 N2 O2'
_chemical_formula_sum            'C26 H44 K2 N2 O2'
_chemical_formula_weight         494.85
_chemical_properties_physical
'Moisture-sensitive, Hygroscopic, Oxygen-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2015-10-18
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Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
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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                81.269(5)
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_cell_angle_gamma                76.025(5)
_cell_formula_units_Z            1
_cell_length_a                   6.1733(4)
_cell_length_b                   10.6514(7)
_cell_length_c                   10.9928(7)
_cell_measurement_reflns_used    8920
_cell_measurement_temperature    123.3
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_cell_measurement_theta_min      3.3945
_cell_volume                     693.19(8)
_computing_cell_refinement
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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_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      123.3
_diffrn_detector_area_resol_mean 16.0727
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9128
_diffrn_measurement_details
;
  1 omega   -8.00   41.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.5833   77.0000 -180.0000 49

  2 omega  -81.00    9.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4426  -77.0000  -60.0000 90

  3 omega  -90.00   -1.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4426  -37.0000  150.0000 89

  4 omega  -47.00   53.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4426   77.0000   60.0000 100

  5 omega  -56.00   42.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.5833  -37.0000 -150.0000 98

  6 omega  -54.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.5833  -77.0000  -30.0000 101

  7 omega   34.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.5833  179.0000   90.0000 59

  8 omega  -94.00  -32.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4426  179.0000   60.0000 62

  9 omega  -90.00    8.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4426  -37.0000  -90.0000 98

 10 omega  -88.00   13.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4426  -77.0000   60.0000 101

 11 omega  -56.00   42.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       16.5833  -37.0000    0.0000 98

 12 omega  -74.00   -2.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.4426  123.0000  165.0000 72
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0700222000
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_diffrn_orient_matrix_UB_21      0.0381990000
_diffrn_orient_matrix_UB_22      -0.0291659000
_diffrn_orient_matrix_UB_23      -0.0528045000
_diffrn_orient_matrix_UB_31      -0.0875300000
_diffrn_orient_matrix_UB_32      -0.0329927000
_diffrn_orient_matrix_UB_33      0.0057426000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14420
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         3.40
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92185
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.1853
_exptl_crystal_description       block
_exptl_crystal_F_000             268.5136
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.8337
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_refine_diff_density_rms         0.0595
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_refine_ls_d_res_low             5.9896
_refine_ls_goodness_of_fit_ref   1.0497
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    40
_refine_ls_number_parameters     165
_refine_ls_number_reflns         3183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0497
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+0.4874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1028
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_reflns_limit_k_max              14
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_reflns_limit_l_min              0
_reflns_number_gt                2839
_reflns_number_total             3183
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c5dt04224k2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7037610--7037614.cif.'
_cod_database_code               7037614
_reflns_odcompleteness_completeness 99.85
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H14c)=Sof(H14d)=Sof(H11c)=Sof(H11d)=Sof(C12)=Sof(H12a)=Sof(H12b)=1-FVAR(1)
 Sof(H14a)=Sof(H14b)=Sof(H11a)=Sof(H11b)=Sof(C13)=Sof(H13a)=Sof(H13b)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C5(H5), C4(H4), C3(H3)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C14(H14a,H14b), C14(H14c,H14d), C11(H11a,H11b), C11(H11c,
 H11d), C13(H13a,H13b), C12(H12a,H12b)
3.c Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C9(H9a,H9b,H9c), C8(H8a,H8b,H8c)
;
_olex2_submission_original_sample_id RMSO2
_olex2_submission_special_instructions 'No special instructions were received'