Stabilization of Calcium Hydride Complexes by Fine Tuning of Amidinate Ligands
Causero, Andrea; Ballmann, Gerd; Pahl, Jürgen; Zijlstra, Harmen; Färber, Christian; Harder, Sjoerd; Organometallics 35 (2016) 3350–; doi:10.1021/acs.organomet.6b00566

data_4088925
_publ_section_title
;
 Stabilization of Calcium Hydride Complexes by Fine Tuning of Amidinate
 Ligands
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              3350
_journal_paper_doi               10.1021/acs.organomet.6b00566
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C39 H71 Ca N3 O Si2'
_chemical_formula_sum            'C39 H71 Ca N3 O Si2'
_chemical_formula_weight         694.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90.146(2)
_cell_angle_beta                 92.606(2)
_cell_angle_gamma                98.163(3)
_cell_formula_units_Z            2
_cell_length_a                   10.6373(4)
_cell_length_b                   12.4259(3)
_cell_length_c                   16.4223(3)
_cell_measurement_reflns_used    24580
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.5730
_cell_measurement_theta_min      4.1060
_cell_volume                     2146.36(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega    0.00   26.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   94.0000  129.4142 26

  2 omega -112.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000 -120.0000 97

  3 omega -112.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000   30.0000 97

  4 omega -114.00  -19.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -38.0000  -60.0000 95

  5 omega  -68.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   57.0000   30.0000 96

  6 omega -114.00  -19.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -38.0000   90.0000 95

  7 omega  -28.00   68.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909  -57.0000 -120.0000 96

  8 omega   23.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909 -125.0000 -180.0000 74

  9 omega    7.00   34.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   87.0000   13.2083 27

 10 omega   14.00   46.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   80.0000  -84.6160 32

 11 omega   17.00   45.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   82.0000   24.8978 28

 12 omega   18.00   46.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   81.0000 -155.8620 28

 13 omega   22.00   49.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  103.4337 27

 14 omega   22.00   49.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000   66.3023 27

 15 omega   22.00   49.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000 -119.9087 27

 16 omega   22.00   49.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000  -46.7816 27

 17 omega   31.00  136.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   77.0000  160.7647 105

 18 omega   35.00  140.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000   54.7615 105

 19 omega   35.00  140.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000   88.6664 105

 20 omega   35.00  140.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000  -68.0990 105

 21 omega   35.00   62.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000  119.9213 27

 22 omega   39.00   65.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000  -18.8960 26

 23 omega   39.00   65.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000  -99.0814 26

 24 omega   40.00   66.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000    7.8247 26

 25 omega   39.00   65.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000 -164.3492 26

 26 omega  118.00  143.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000  -99.0814 25

 27 omega  103.00  129.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000  -18.8960 26

 28 omega   40.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000  134.6192 43

 29 omega  117.00  143.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000 -141.4328 26

 30 omega   40.00   65.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000 -141.4328 25

 31 omega   43.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000  -43.2000 26

 32 omega   44.00   72.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   76.0000  -90.9031 28

 33 omega   78.00  105.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000   90.0000 27

 34 omega   35.00  116.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000   30.0000 81

 35 omega   76.00  172.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000 -180.0000 96

 36 omega   82.00  107.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000  120.0000 25

 37 omega   84.00  111.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000   30.0000 27

 38 omega   78.00  117.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000  150.0000 39

 39 omega   29.00   83.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000  -60.0000 54

 40 omega   75.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000    0.0000 103

 41 omega   35.00  112.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000 -150.0000 77

 42 omega   75.00  153.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000  -60.0000 78

 43 omega   76.00  151.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000 -120.0000 75

 44 omega  152.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000 -120.0000 26

 45 omega   78.00  119.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000    0.0000 41

 46 omega   75.00  148.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000   60.0000 73

 47 omega  115.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000   30.0000 62

 48 omega   40.00  116.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000   30.0000 76

 49 omega   77.00  104.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000   30.0000 27

 50 omega   75.00  101.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000  -30.0000 26

 51 omega  121.00  147.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000  -30.0000 26

 52 omega   27.00  108.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000 -150.0000 81

 53 omega   75.00  140.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000 -150.0000 65

 54 omega   32.00  108.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000   30.0000 76

 55 omega  130.00  156.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000  120.0000 26

 56 omega   75.00  173.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000   90.0000 98

 57 omega   79.00  111.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000   60.0000 32

 58 omega   75.00  149.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000  150.0000 74

 59 omega   75.00  150.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000  -90.0000 75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0559835000
_diffrn_orient_matrix_UB_12      0.0834750000
_diffrn_orient_matrix_UB_13      -0.0626076000
_diffrn_orient_matrix_UB_21      0.1204346000
_diffrn_orient_matrix_UB_22      0.0284717000
_diffrn_orient_matrix_UB_23      0.0559543000
_diffrn_orient_matrix_UB_31      0.0617557000
_diffrn_orient_matrix_UB_32      -0.0889382000
_diffrn_orient_matrix_UB_33      -0.0420533000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16049
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.836
_diffrn_reflns_theta_min         3.594
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.014
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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    1.074
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.3255
_exptl_crystal_size_mid          0.1707
_exptl_crystal_size_min          0.1241
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         16049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+0.0500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14047
_reflns_number_total             16049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00566_si_009.cif
_cod_data_source_block           hasj160321a_twin1_hklf4
_cod_database_code               4088925
_chemical_oxdiff_formula         'C H N O Ca Si I '
_diffrn_oxdiff_twin_integration_method simultaneous
_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:
 C24(H24), C15(H15), C12(H12), C27(H27)
2.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C36(H36A,H36B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C22(H22), C10(H10), C20(H20), C9(H9), C21(H21)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C3(H3A,H3B,H3C), C33(H33A,H33B,H33C), C31(H31A,H31B,
 H31C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C35(H35A,H35B,H35C), C17(H17A,
 H17B,H17C), C13(H13A,H13B,H13C), C30(H30A,H30B,H30C), C16(H16A,H16B,H16C),
 C39(H39A,H39B,H39C), C29(H29A,H29B,H29C), C37(H37A,H37B,H37C), C28(H28A,H28B,
 H28C)
;
_shelx_res_checksum              4874
_shelx_hkl_checksum              87858
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id hasj160321a
_olex2_submission_special_instructions 'No special instructions were received'