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_4088923
_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         'C50 H72 Ca N4 O'
_chemical_formula_sum            'C50 H72 Ca N4 O'
_chemical_formula_weight         785.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-11-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.4699(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.12062(13)
_cell_length_b                   16.59171(16)
_cell_length_c                   22.9746(2)
_cell_measurement_reflns_used    30876
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.6140
_cell_measurement_theta_min      3.2660
_cell_volume                     4620.08(8)
_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, 2008)'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -68.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   57.0000  -90.0000 96

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

  3 omega  -32.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909  -77.0000    0.0000 105

  4 omega   32.00  137.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000 -180.0000 105

  5 omega   31.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000 -150.0000 60

  6 omega   31.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  -60.0000 60

  7 omega   34.00  121.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000    0.0000 87

  8 omega   25.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000   90.0000 84

  9 omega   82.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000  120.0000 95

 10 omega   35.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000   90.0000 63

 11 omega   32.00  137.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000    0.0000 105

 12 omega   31.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  -30.0000 60

 13 omega   26.00  151.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -15.0000   90.0000 125

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

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

 16 omega  -50.00   31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   38.0000  150.0000 81

 17 omega -112.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000 -150.0000 97

 18 omega   78.00  176.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000 -180.0000 98

 19 omega   78.00  176.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000  -30.0000 98

 20 omega   82.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   30.0000  -90.0000 96
;
_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      0.0241833000
_diffrn_orient_matrix_UB_12      0.0660545000
_diffrn_orient_matrix_UB_13      0.0454889000
_diffrn_orient_matrix_UB_21      0.0914105000
_diffrn_orient_matrix_UB_22      0.0342151000
_diffrn_orient_matrix_UB_23      -0.0390898000
_diffrn_orient_matrix_UB_31      -0.0849598000
_diffrn_orient_matrix_UB_32      0.0556041000
_diffrn_orient_matrix_UB_33      -0.0299400000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            49263
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.116
_diffrn_reflns_theta_min         3.286
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.458
_exptl_absorpt_correction_T_max  1.00000
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_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
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_exptl_crystal_description       block
_exptl_crystal_F_000             1712
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_exptl_crystal_size_mid          0.3125
_exptl_crystal_size_min          0.1885
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
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_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.0376
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+1.3180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8089
_reflns_number_total             8433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00566_si_005.cif
_cod_data_source_block           hasj151102a
_cod_original_cell_volume        4620.09(8)
_cod_database_code               4088923
_chemical_oxdiff_formula         'C H N O Si Ca'
_reflns_odcompleteness_completeness 99.94
_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. Others
 Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C25B)=Sof(H25D)=Sof(H25E)=
 Sof(H25F)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C24A)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
 Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(H3BC)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(H4BC)=
 Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(H2BC)=1-FVAR(2)
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C47(H47A,H47B)
3.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C18(H18), C38(H38), C7(H7), C40(H40), C29(H29), C16(H16), C9(H9)
3.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C20(H20A,H20B,H20C), C42(H42A,H42B,H42C), C34(H34A,H34B,
 H34C), C11(H11A,H11B,H11C), C21(H21A,H21B,H21C), C48(H48A,H48B,H48C), C22(H22A,
 H22B,H22C), C43(H43A,H43B,H43C), C46(H46A,H46B,H46C), C35(H35A,H35B,H35C),
 C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C25A(H25A,H25B,H25C), C44(H44A,H44B,
 H44C), C24A(H24A,H24B,H24C), C4A(H4AA,H4AB,H4AC), C2A(H2AA,H2AB,H2AC),
 C3A(H3AA,H3AB,H3AC), C26A(H26A,H26B,H26C), C26B(H26D,H26E,H26F), C25B(H25D,
 H25E,H25F), C24B(H24D,H24E,H24F), C3B(H3BA,H3BB,H3BC), C4B(H4BA,H4BB,H4BC),
 C2B(H2BA,H2BB,H2BC)
;
_shelx_res_checksum              34016
_shelx_hkl_checksum              93738
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-11-02
_olex2_submission_original_sample_id HASJ151102a
_olex2_submission_special_instructions 'No special instructions were received'