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_4088932
_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         'C70 H100 Ca2 N4, 4(C6 H6)'
_chemical_formula_sum            'C94 H124 Ca2 N4'
_chemical_formula_weight         1390.12
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                83.3598(15)
_cell_angle_beta                 87.9438(15)
_cell_angle_gamma                69.2211(18)
_cell_formula_units_Z            1
_cell_length_a                   10.4550(2)
_cell_length_b                   10.5225(2)
_cell_length_c                   19.8508(3)
_cell_measurement_reflns_used    26883
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.6160
_cell_measurement_theta_min      4.4910
_cell_volume                     2028.07(7)
_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      N~2~
_diffrn_ambient_temperature      100.00(10)
_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 0.999
_diffrn_measurement_details
;
  1 omega    1.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       38.0000   92.0000  160.5099 27

  2 omega -120.00   -5.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -19.0000 -180.0000 115

  3 omega -112.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000   90.0000 97

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

  5 omega   19.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909   38.0000  -30.0000 95

  6 omega   23.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909 -125.0000   60.0000 74

  7 omega  -31.00   64.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909  -38.0000   60.0000 95

  8 omega   15.00  112.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909   57.0000   90.0000 97

  9 omega   13.00   45.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   82.0000  -27.4258 32

 10 omega   14.00   49.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       46.0000   78.0000   62.4325 35

 11 omega   17.00   45.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   82.0000   31.2664 28

 12 omega   18.00   47.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  -74.4647 29

 13 omega   17.00   45.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   82.0000 -145.2904 28

 14 omega   17.00   45.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   82.0000  117.7271 28

 15 omega   22.00   49.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   78.0000 -169.9371 27

 16 omega   27.00  132.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000   77.0000  133.9418 105

 17 omega   35.00  139.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   75.0000  167.8308 104

 18 omega   35.00  140.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   77.0000   21.8154 105

 19 omega   35.00  139.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   75.0000   73.0210 104

 20 omega   35.00  139.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       66.0000   76.0000  -53.8478 104

 21 omega   39.00  144.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000 -175.0284 105

 22 omega   39.00  144.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000   -7.3228 105

 23 omega   39.00  140.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000  -38.1485 101

 24 omega   39.00   65.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   75.0000 -120.6471 26

 25 omega   39.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   76.0000  -88.5934 31

 26 omega   39.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       70.0000   77.0000  131.2956 31

 27 omega   43.00   84.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000   78.4512 41

 28 omega  107.00  148.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000   78.4512 41

 29 omega   45.00  135.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000  120.0000 90

 30 omega   75.00  172.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000  -30.0000 97

 31 omega   75.00  170.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000   60.0000 95

 32 omega   78.00  108.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000  150.0000 30

 33 omega  150.00  177.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000 -120.0000 27

 34 omega   75.00  149.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000 -120.0000 74

 35 omega   75.00  176.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000    0.0000 101

 36 omega  113.00  175.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000  -60.0000 62

 37 omega   75.00  164.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000  -90.0000 89

 38 omega   27.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000   60.0000 82

 39 omega   75.00  167.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000  150.0000 92

 40 omega  114.00  149.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000  120.0000 35

 41 omega   75.00  174.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000 -150.0000 99

 42 omega   76.00  101.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000  -60.0000 25

 43 omega   75.00  101.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000  120.0000 26

 44 omega   78.00  105.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000   30.0000 27

 45 omega   76.00  143.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000   30.0000 67

 46 omega   82.00  114.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000  -30.0000 32

 47 omega   75.00  171.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000   90.0000 96

 48 omega   75.00  151.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000 -180.0000 76

 49 omega  138.00  174.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000   60.0000 36

 50 omega   34.00  120.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000  -60.0000 86

 51 omega   26.00  103.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000    0.0000 77
;
_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      0.1067581000
_diffrn_orient_matrix_UB_12      -0.1439728000
_diffrn_orient_matrix_UB_13      0.0181240000
_diffrn_orient_matrix_UB_21      -0.0725353000
_diffrn_orient_matrix_UB_22      -0.0128200000
_diffrn_orient_matrix_UB_23      0.0680176000
_diffrn_orient_matrix_UB_31      -0.0904483000
_diffrn_orient_matrix_UB_32      -0.0626866000
_diffrn_orient_matrix_UB_33      -0.0339086000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0728
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41056
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.093
_diffrn_reflns_theta_min         4.485
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.569
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.138
_exptl_crystal_description       block
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.4655
_exptl_crystal_size_mid          0.1638
_exptl_crystal_size_min          0.1088
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         7410
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0884P)^2^+1.6026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1570
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7002
_reflns_number_total             7410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00566_si_007.cif
_cod_data_source_block           hasj151204b
_cod_original_cell_volume        2028.06(7)
_cod_database_code               4088932
_chemical_oxdiff_formula         'C H N Ca'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.96
_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. Rigid body (RIGU) restrains
 C44, C43, C42, C47, C46, C45
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C46A)=Sof(H46A)=Sof(C47A)=Sof(H47A)=Sof(C42A)=Sof(H42A)=Sof(C43A)=
 Sof(H43A)=Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(H45A)=1-FVAR(1)
 Sof(C44)=Sof(H44)=Sof(C43)=Sof(H43)=Sof(C42)=Sof(H42)=Sof(C47)=Sof(H47)=
 Sof(C46)=Sof(H46)=Sof(C45)=Sof(H45)=FVAR(1)
 Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39A)=Sof(C40A)=
 Sof(H40A)=Sof(C41A)=Sof(H41A)=Sof(C36A)=Sof(H36A)=1-FVAR(2)
 Sof(C40)=Sof(H40)=Sof(C39)=Sof(H39)=Sof(C38)=Sof(H38)=Sof(C41)=Sof(H41)=
 Sof(C37)=Sof(H37)=Sof(C36)=Sof(H36)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C33(H33), C18(H18), C30(H30), C19(H19), C20(H20)
4.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C22(H22A,H22B), C17(H17A,H17B), C16(H16A,H16B), C23(H23A,
 H23B), C21(H21A,H21B)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C4(H4), C28(H28), C27(H27), C26(H26), C44(H44), C43(H43),
 C42(H42), C47(H47), C46(H46), C45(H45), C46A(H46A), C47A(H47A), C42A(H42A),
 C43A(H43A), C44A(H44A), C45A(H45A), C40(H40), C39(H39), C38(H38), C41(H41),
 C37(H37), C36(H36), C37A(H37A), C38A(H38A), C39A(H39A), C40A(H40A), C41A(H41A),
  C36A(H36A)
4.d Fitted hexagon refined as free rotating group:
 C44(C43,C42,C47,C46,C45), C46A(C47A,C42A,C43A,C44A,C45A), C37A(C38A,C39A,C40A,
 C41A,C36A)
4.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C35(H35A,H35B,H35C), C9(H9A,H9B,H9C), C11(H11A,H11B,
 H11C), C8(H8A,H8B,H8C), C34(H34A,H34B,H34C), C32(H32A,H32B,H32C), C31(H31A,
 H31B,H31C)
;
_shelx_res_checksum              84552
_shelx_hkl_checksum              22552
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-12-04
_olex2_submission_special_instructions 'No special instructions were received'