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_4088929
_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         'C41 H67 Ca N3 Si2'
_chemical_formula_sum            'C41 H67 Ca N3 Si2'
_chemical_formula_weight         698.23
_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             2016-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.2021(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.87724(17)
_cell_length_b                   12.3264(2)
_cell_length_c                   33.7986(7)
_cell_measurement_reflns_used    7244
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.5510
_cell_measurement_theta_min      3.7800
_cell_volume                     4111.97(13)
_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
_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  -64.00   30.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   77.0000    0.0000 94

  2 omega -105.00  -27.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -38.0000 -120.0000 78

  3 omega -113.00  -70.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -38.0000  -30.0000 43

  4 omega  129.00  159.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000    0.0000 30

  5 omega   78.00  165.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000   60.0000 87

  6 omega   50.00  137.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000  -90.0000 87

  7 omega   82.00  170.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000 -180.0000 88

  8 omega   42.00  131.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -61.0000   90.0000 89
;
_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      -0.0547023000
_diffrn_orient_matrix_UB_12      -0.1115608000
_diffrn_orient_matrix_UB_13      -0.0134944000
_diffrn_orient_matrix_UB_21      -0.1438738000
_diffrn_orient_matrix_UB_22      0.0478782000
_diffrn_orient_matrix_UB_23      -0.0044930000
_diffrn_orient_matrix_UB_31      0.0256015000
_diffrn_orient_matrix_UB_32      0.0296694000
_diffrn_orient_matrix_UB_33      -0.0433584000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            14210
_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         68.118
_diffrn_reflns_theta_min         3.817
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.090
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.959
_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    1.128
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.1652
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.1011
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         7446
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0800P)^2^+1.9770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6633
_reflns_number_total             7446
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00566_si_008.cif
_cod_data_source_block           hasj160303a
_cod_original_cell_volume        4111.98(14)
_cod_database_code               4088929
_chemical_oxdiff_formula         'C H N O Si Ca'
_reflns_odcompleteness_completeness 99.54
_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.a Ternary CH refined with riding coordinates:
 C21(H21), C18(H18), C6(H6), C10(H10), C8(H8), C33(H33), C30(H30)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C3(H3A,H3B), C9(H9A,H9B), C7(H7A,H7B), C11(H11A,H11B)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C14(H14), C15(H15), C28(H28), C26(H26), C27(H27)
2.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C22(H22A,H22B,
 H22C), C34(H34A,H34B,H34C), C40(H40A,H40B,H40C), C35(H35A,H35B,H35C), C31(H31A,
 H31B,H31C), C41(H41A,H41B,H41C), C39(H39A,H39B,H39C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C), C32(H32A,H32B,H32C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              58912
_shelx_hkl_checksum              61767
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-03-03
_olex2_submission_original_sample_id hasj160303a
_olex2_submission_special_instructions 'No special instructions were received'