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_4088927
_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         'C40 H73 Ca N3 O Si2'
_chemical_formula_sum            'C40 H73 Ca N3 O Si2'
_chemical_formula_weight         708.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 94.156(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7482(7)
_cell_length_b                   18.0397(7)
_cell_length_c                   16.8077(7)
_cell_measurement_reflns_used    7398
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.3830
_cell_measurement_theta_min      3.8560
_cell_volume                     4460.0(3)
_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 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega  -50.00   31.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   38.0000  120.0000 81

  2 omega -112.00  -15.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000  -30.0000 97

  3 omega   83.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   30.0000    0.0000 95

  4 omega   99.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000 -120.0000 77

  5 omega   34.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000   90.0000 56

  6 omega   36.00   73.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000   30.0000 37

  7 omega   33.00   96.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000  -90.0000 63

  8 omega   31.00   80.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000 -180.0000 49
;
_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      -0.0488232000
_diffrn_orient_matrix_UB_12      0.0310726000
_diffrn_orient_matrix_UB_13      0.0707153000
_diffrn_orient_matrix_UB_21      -0.0900602000
_diffrn_orient_matrix_UB_22      -0.0345117000
_diffrn_orient_matrix_UB_23      -0.0346001000
_diffrn_orient_matrix_UB_31      0.0221568000
_diffrn_orient_matrix_UB_32      -0.0716279000
_diffrn_orient_matrix_UB_33      0.0473683000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14692
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.115
_diffrn_reflns_theta_min         3.004
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.947
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.954
_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    1.055
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.1961
_exptl_crystal_size_mid          0.0896
_exptl_crystal_size_min          0.0687
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         8068
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0645
_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^)+(0.1150P)^2^+1.6300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1716
_refine_ls_wR_factor_ref         0.1965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6810
_reflns_number_total             8068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00566_si_004.cif
_cod_data_source_block           hasj151021a
_cod_database_code               4088927
_chemical_oxdiff_formula         'C H N Ca Si O'
_reflns_odcompleteness_completeness 98.99
_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. Restrained distances
 C40A-C39A
 1.54 with sigma of 0.01
 C39A-O1
 1.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O1) = Uanis(C39A) = Uanis(C40A)
4. Rigid body (RIGU) restrains
 C38A, C37A, O1, C39A, C40A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=
 Sof(C39A)=Sof(H39C)=Sof(H39D)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(1)
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=Sof(H40C)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(1)
 Sof(H28A)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C29A)=Sof(H29D)=
 Sof(H29E)=Sof(H29F)=1-FVAR(2)
 Sof(H28)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)=
 Sof(H30C)=FVAR(2)
 Sof(H16A)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C17A)=Sof(H17D)=
 Sof(H17E)=Sof(H17F)=1-FVAR(3)
 Sof(H16)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C17)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C16(H16A), C25(H25), C28(H28), C28(H28A)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C39(H39A,H39B), C37(H37A,H37B), C37A(H37C,H37D), C39A(H39C,H39D)
6.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C9(H9), C23(H23), C22(H22), C11(H11), C10(H10)
6.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C35(H35A,H35B,H35C),
 C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C15(H15A,H15B,H15C), C14(H14A,H14B,
 H14C), C36(H36A,H36B,H36C), C34(H34A,H34B,H34C), C18(H18A,H18B,H18C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C29(H29A,H29B,H29C), C17(H17A,H17B,H17C),
 C33(H33A,H33B,H33C), C30(H30A,H30B,H30C), C40(H40A,H40B,H40C), C38(H38A,H38B,
 H38C), C38A(H38D,H38E,H38F), C40A(H40D,H40E,H40F), C30A(H30D,H30E,H30F),
 C29A(H29D,H29E,H29F), C18A(H18D,H18E,H18F), C17A(H17D,H17E,H17F)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-10-21
_olex2_submission_special_instructions 'No special instructions were received'