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_4088924
_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         'C64 H110 Ca2 N6 Si4'
_chemical_formula_sum            'C64 H110 Ca2 N6 Si4'
_chemical_formula_weight         1156.09
_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                102.6714(13)
_cell_angle_beta                 94.2421(13)
_cell_angle_gamma                106.0615(14)
_cell_formula_units_Z            2
_cell_length_a                   11.78345(19)
_cell_length_b                   15.5905(2)
_cell_length_c                   23.5944(4)
_cell_measurement_reflns_used    27608
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.7320
_cell_measurement_theta_min      3.9730
_cell_volume                     4021.74(12)
_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)'
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_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
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_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega  -73.00   32.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   77.0000   90.0000 105

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

  3 omega   10.00  116.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909   77.0000 -180.0000 106

  4 omega   35.00  130.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000 -150.0000 95

  5 omega   34.00  121.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000   90.0000 87

  6 omega   82.00  178.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   30.0000  -90.0000 96

  7 omega   31.00  130.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000   90.0000 99

  8 omega   32.00  137.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000 -120.0000 105

  9 omega   25.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000 -150.0000 84

 10 omega   82.00  177.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000  -30.0000 95

 11 omega   25.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000  150.0000 84

 12 omega   94.00  178.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000 -150.0000 84

 13 omega   31.00  130.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  -60.0000 99

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

 15 omega -112.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000    0.0000 97

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

 17 omega    1.00   82.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909  -99.0000 -150.0000 81

 18 omega   78.00  176.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000 -180.0000 98

 19 omega   61.00  178.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   15.0000  120.0000 117
;
_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      -0.0193287000
_diffrn_orient_matrix_UB_12      -0.0370308000
_diffrn_orient_matrix_UB_13      -0.0672290000
_diffrn_orient_matrix_UB_21      0.1332609000
_diffrn_orient_matrix_UB_22      0.0069695000
_diffrn_orient_matrix_UB_23      0.0017434000
_diffrn_orient_matrix_UB_31      -0.0277026000
_diffrn_orient_matrix_UB_32      -0.0992981000
_diffrn_orient_matrix_UB_33      0.0070930000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            43916
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.114
_diffrn_reflns_theta_min         4.002
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.056
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.909
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.955
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.3767
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.1763
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         14614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0640P)^2^+1.9610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1136
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13368
_reflns_number_total             14614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00566_si_011.cif
_cod_data_source_block           hasj160412a
_cod_original_cell_volume        4021.75(11)
_cod_database_code               4088924
_chemical_oxdiff_formula         'C H N Ca Si O '
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.96
_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.a Ternary CH refined with riding coordinates:
 C9(H9), C38(H38), C12(H12), C35(H35), C21(H21), C47(H47), C50(H50), C24(H24)
2.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C33(H33), C5(H5), C32(H32), C7(H7), C6(H6), C45(H45), C17(H17),
 C19(H19), C43(H43), C18(H18), C44(H44)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C28(H28A,H28B,H28C), C55(H55A,H55B,H55C), C39(H39A,H39B,
 H39C), C54(H54A,H54B,H54C), C53(H53A,H53B,H53C), C57(H57A,H57B,H57C), C62(H62A,
 H62B,H62C), C61(H61A,H61B,H61C), C40(H40A,H40B,H40C), C63(H63A,H63B,H63C),
 C37(H37A,H37B,H37C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C59(H59A,H59B,
 H59C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C11(H11A,H11B,H11C), C64(H64A,
 H64B,H64C), C36(H36A,H36B,H36C), C48(H48A,H48B,H48C), C14(H14A,H14B,H14C),
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C49(H49A,H49B,H49C), C52(H52A,H52B,
 H52C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C51(H51A,H51B,H51C), C60(H60A,
 H60B,H60C)
;
_shelx_res_checksum              36348
_shelx_hkl_checksum              31589
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-04-12
_olex2_submission_original_sample_id hasj160412a
_olex2_submission_special_instructions 'No special instructions were received'