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_4088928
_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         '2(C38 H59 Ca N3 Si2), 4(C7 H8)'
_chemical_formula_sum            'C104 H150 Ca2 N6 Si4'
_chemical_formula_weight         1676.81
_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             2016-05-25
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                110.503(2)
_cell_angle_beta                 102.6180(10)
_cell_angle_gamma                100.0220(10)
_cell_formula_units_Z            2
_cell_length_a                   16.3967(2)
_cell_length_b                   16.4260(3)
_cell_length_c                   21.1559(4)
_cell_measurement_reflns_used    39467
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.7680
_cell_measurement_theta_min      3.5190
_cell_volume                     5008.65(17)
_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 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -50.00   31.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   38.0000  -30.0000 81

  2 omega  -50.00   31.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   38.0000 -180.0000 81

  3 omega  -96.00   -2.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  125.0000 -180.0000 94

  4 omega -112.00  -15.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000   30.0000 97

  5 omega   32.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205  -30.0000   60.0000 59

  6 omega   32.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205  -30.0000 -180.0000 59

  7 omega   33.00  138.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205  -77.0000  -60.0000 105

  8 omega   35.00  122.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205 -125.0000  150.0000 87

  9 omega   25.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205  -94.0000 -120.0000 84

 10 omega   27.00  152.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205  -15.0000  -90.0000 125

 11 omega   75.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205   77.0000    0.0000 103

 12 omega   94.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205  125.0000  -60.0000 84

 13 omega   79.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205   61.0000   90.0000 98

 14 omega -112.00  -15.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000  120.0000 97

 15 omega -116.00  -10.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -77.0000 -150.0000 106

 16 omega -112.00  -15.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000  -60.0000 97

 17 omega    1.00   82.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909  -99.0000   60.0000 81

 18 omega   79.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205   61.0000  120.0000 98

 19 omega   79.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205   61.0000 -150.0000 98

 20 omega   79.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205   61.0000  150.0000 98

 21 omega   79.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205   61.0000 -120.0000 98

 22 omega   83.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205   30.0000  -60.0000 95

 23 omega   79.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205   61.0000 -180.0000 98

 24 omega   79.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205   61.0000  -30.0000 98

 25 omega   79.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205   61.0000   60.0000 98

 26 omega -116.00  -10.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -77.0000  -90.0000 106

 27 omega -116.00  -10.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -77.0000  120.0000 106

 28 omega -114.00  -19.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -38.0000  150.0000 95

 29 omega -116.00  -10.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -77.0000   30.0000 106

 30 omega   75.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205   77.0000   30.0000 103

 31 omega   75.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205   77.0000  -30.0000 103

 32 omega   79.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.6205   61.0000  -60.0000 98
;
_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      -0.0951992000
_diffrn_orient_matrix_UB_12      -0.0422800000
_diffrn_orient_matrix_UB_13      -0.0472820000
_diffrn_orient_matrix_UB_21      -0.0180593000
_diffrn_orient_matrix_UB_22      0.0929586000
_diffrn_orient_matrix_UB_23      0.0285225000
_diffrn_orient_matrix_UB_31      0.0251801000
_diffrn_orient_matrix_UB_32      0.0202929000
_diffrn_orient_matrix_UB_33      -0.0600484000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32796
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.217
_diffrn_reflns_theta_min         2.872
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.796
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.964
_exptl_absorpt_correction_type   analytical
_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) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.426
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.1309
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1284
_refine_ls_number_reflns         32796
_refine_ls_number_restraints     191
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0594
_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^)+(0.1350P)^2^+0.4500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29447
_reflns_number_total             32796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00566_si_002.cif
_cod_data_source_block           hasj150309c_twin1_hklf4
_cod_original_cell_volume        5008.65(16)
_cod_database_code               4088928
_chemical_oxdiff_formula         'Ca N C H '
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C49A-C48A
 1.54 with sigma of 0.01
 C50A-C48A
 1.54 with sigma of 0.01
 C65A-C60A
 1.54 with sigma of 0.01
 C68A-C70A
 1.54 with sigma of 0.01
 C68A-C69A
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C60) = Uanis(C70A)
Uanis(C65) = Uanis(C68A)
4. Rigid body (RIGU) restrains
 C68A, C65A, C45A, C44A, C43A, C42A, C41A, C40A, C39A, N4A, N5A, C59A, C64A,
 C63A, C62A, C61A, C60A, C48A, C50A, C49A, C46A, C47A, C67A, C66A, C70A, C69A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N4(0.8) N5(0.8) C68A(0.2) H68A(0.2) C60(0.8) C64(0.8) C65A(0.2)
 H65A(0.2) C67(0.8) H67A(0.8) H67B(0.8) H67C(0.8) C63(0.8) H63(0.8) C66(0.8)
 H66A(0.8) H66B(0.8) H66C(0.8) C45(0.8) H45(0.8) C61(0.8) H61(0.8) C40(0.8)
 C45A(0.2) H45A(0.2) C59(0.8) C62(0.8) H62(0.8) C69(0.8) H69A(0.8) H69B(0.8)
 H69C(0.8) C70(0.8) H70A(0.8) H70B(0.8) H70C(0.8) C39(0.8) C44(0.8) C41(0.8)
 H41(0.8) C49(0.8) H49A(0.8) H49B(0.8) H49C(0.8) C43(0.8) H43(0.8) C46(0.8)
 H46A(0.8) H46B(0.8) H46C(0.8) C42(0.8) H42(0.8) C44A(0.2) C43A(0.2) H43A(0.2)
 C42A(0.2) H42A(0.2) C41A(0.2) H41A(0.2) C40A(0.2) C39A(0.2) C50(0.8) H50A(0.8)
 H50B(0.8) H50C(0.8) N4A(0.2) N5A(0.2) C59A(0.2) C64A(0.2) C63A(0.2) H63A(0.2)
 C62A(0.2) H62A(0.2) C61A(0.2) H61A(0.2) C60A(0.2) C47(0.8) H47A(0.8) H47B(0.8)
 H47C(0.8) C48A(0.2) H48A(0.2) C50A(0.2) H50D(0.2) H50E(0.2) H50F(0.2)
 C49A(0.2) H49D(0.2) H49E(0.2) H49F(0.2) C46A(0.2) H46D(0.2) H46E(0.2)
 H46F(0.2) C47A(0.2) H47D(0.2) H47E(0.2) H47F(0.2) C68(0.8) H68(0.8) C67A(0.2)
 H67D(0.2) H67E(0.2) H67F(0.2) C66A(0.2) H66D(0.2) H66E(0.2) H66F(0.2) C48(0.8)
 H48(0.8) C70A(0.2) H70D(0.2) H70E(0.2) H70F(0.2) C69A(0.2) H69D(0.2) H69E(0.2)
 H69F(0.2) C65(0.8) H65(0.8)
6.a Ternary CH refined with riding coordinates:
 C10(H10), C27(H27), C68A(H68A), C30(H30), C7(H7), C65A(H65A), C45(H45),
 C45A(H45A), C48A(H48A), C68(H68), C48(H48), C65(H65)
6.b Me refined with riding coordinates:
 C69A(H69D,H69E,H69F)
6.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C18(H18), C16(H16), C54(H54), C23(H23), C19(H19), C56(H56), C4(H4),
 C24(H24), C3(H3), C5(H5), C53(H53), C25(H25), C57(H57), C63(H63), C102(H102),
 C61(H61), C91(H91), C94(H94), C95(H95), C100(H100), C98(H98), C62(H62),
 C93(H93), C101(H101), C99(H99), C92(H92), C41(H41), C77(H77), C43(H43),
 C42(H42), C43A(H43A), C42A(H42A), C41A(H41A), C88(H88), C84(H84), C80(H80),
 C78(H78), C81(H81), C79(H79), C85(H85), C86(H86), C87(H87), C63A(H63A),
 C62A(H62A), C61A(H61A)
6.d Fitted hexagon refined as free rotating group:
 C44A(C43A,C42A,C41A,C40A,C39A), C59A(C64A,C63A,C62A,C61A,C60A)
6.e Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C20(H20A,H20B,H20C), C38(H38A,H38B,H38C), C31(H31A,H31B,
 H31C), C35(H35A,H35B,H35C), C8(H8A,H8B,H8C), C74(H74A,H74B,H74C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C73(H73A,H73B,H73C), C72(H72A,H72B,H72C),
 C11(H11A,H11B,H11C), C28(H28A,H28B,H28C), C71(H71A,H71B,H71C), C67(H67A,H67B,
 H67C), C29(H29A,H29B,H29C), C66(H66A,H66B,H66C), C33(H33A,H33B,H33C), C9(H9A,
 H9B,H9C), C12(H12A,H12B,H12C), C76(H76A,H76B,H76C), C75(H75A,H75B,H75C),
 C58(H58A,H58B,H58C), C69(H69A,H69B,H69C), C34(H34A,H34B,H34C), C70(H70A,H70B,
 H70C), C49(H49A,H49B,H49C), C104(H10A,H10B,H10C), C46(H46A,H46B,H46C),
 C97(H97A,H97B,H97C), C50(H50A,H50B,H50C), C83(H83A,H83B,H83C), C90(H90A,H90B,
 H90C), C47(H47A,H47B,H47C), C50A(H50D,H50E,H50F), C49A(H49D,H49E,H49F),
 C46A(H46D,H46E,H46F), C47A(H47D,H47E,H47F), C67A(H67D,H67E,H67F), C66A(H66D,
 H66E,H66F), C70A(H70D,H70E,H70F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'