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_4088926
_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         '2(C45 H75 Ca N3 O Si2), C6 H6'
_chemical_formula_sum            'C96 H156 Ca2 N6 O2 Si4'
_chemical_formula_weight         1618.78
_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             2016-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.0355(13)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   31.2740(5)
_cell_length_b                   22.9849(2)
_cell_length_c                   21.3045(2)
_cell_measurement_reflns_used    23619
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.4730
_cell_measurement_theta_min      3.4960
_cell_volume                     14561.8(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      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 0.993
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -69.00   29.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   77.0000  150.0000 98

  2 omega -112.00  -15.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000  -30.0000 97

  3 omega   42.00   70.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -61.0000   90.0000 28

  4 omega   88.00  134.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -61.0000   90.0000 46

  5 omega   84.00  176.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   61.0000   90.0000 92

  6 omega  113.00  176.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000    0.0000 63

  7 omega   76.00  174.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000   30.0000 98

  8 omega   32.00  130.00   1.0000   14.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000  -30.0000 98
;
_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      0.0063016000
_diffrn_orient_matrix_UB_12      0.0583255000
_diffrn_orient_matrix_UB_13      -0.0317066000
_diffrn_orient_matrix_UB_21      0.0231413000
_diffrn_orient_matrix_UB_22      0.0256002000
_diffrn_orient_matrix_UB_23      0.0690313000
_diffrn_orient_matrix_UB_31      0.0458878000
_diffrn_orient_matrix_UB_32      -0.0208399000
_diffrn_orient_matrix_UB_33      -0.0039801000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            53201
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.116
_diffrn_reflns_theta_min         2.908
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.848
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.981
_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    1.108
_exptl_crystal_description       block
_exptl_crystal_F_000             5316
_exptl_crystal_size_max          0.3257
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.0736
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1528
_refine_ls_number_reflns         26403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0610P)^2^+5.2090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22467
_reflns_number_total             26403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00566_si_012.cif
_cod_data_source_block           hasj160706b
_cod_database_code               4088926
_chemical_oxdiff_formula         'C H N O Si Ca'
_reflns_odcompleteness_completeness 99.39
_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:
 C98(H98), C116(H116), C59(H59), C111(H111), C123(H123), C66(H66), C78(H78),
 C53(H53), C104(H104), C71(H71), C55(H55), C6(H6), C100(H100), C26(H26),
 C14(H14), C96(H96), C33(H33), C51(H51), C21(H21), C8(H8), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C93(H93A,H93B), C48(H48A,H48B), C49(H49A,H49B), C45(H45A,H45B), C94(H94A,
 H94B), C135(H13A,H13B), C97(H97A,H97B), C95(H95A,H95B), C54(H54A,H54B),
 C42(H42A,H42B), C99(H99A,H99B), C87(H87A,H87B), C44(H44A,H44B), C134(H13C,
 H13D), C43(H43A,H43B), C50(H50A,H50B), C132(H13E,H13F), C56(H56A,H56B),
 C101(H10A,H10B), C52(H52A,H52B), C5(H5A,H5B), C4(H4A,H4B), C133(H13M,H13N),
 C7(H7A,H7B), C3(H3A,H3B), C88(H88A,H88B), C90(H90A,H90B), C9(H9A,H9B),
 C11(H11M,H11N), C89(H89A,H89B)
2.c Aromatic/amide H refined with riding coordinates:
 C109(H109), C121(H121), C120(H120), C64(H64), C76(H76), C62(H62), C107(H107),
 C119(H119), C108(H108), C31(H31), C75(H75), C29(H29), C63(H63), C74(H74),
 C30(H30), C138(H138), C17(H17), C137(H137), C141(H141), C140(H140), C143(H143),
  C139(H139), C136(H136), C19(H19), C144(H144), C18(H18), C142(H142)
2.d Idealised Me refined as rotating group:
 C126(H12A,H12B,H12C), C85(H85A,H85B,H85C), C67(H67A,H67B,H67C), C128(H12D,
 H12E,H12F), C124(H12G,H12H,H12I), C39(H39A,H39B,H39C), C80(H80A,H80B,H80C),
 C40(H40A,H40B,H40C), C118(H11A,H11B,H11C), C79(H79A,H79B,H79C), C125(H12J,H12K,
 H12L), C112(H11D,H11E,H11F), C28(H28A,H28B,H28C), C117(H11G,H11H,H11I),
 C113(H11J,H11K,H11L), C60(H60A,H60B,H60C), C84(H84A,H84B,H84C), C127(H12M,H12N,
 H12O), C131(H13G,H13H,H13I), C68(H68A,H68B,H68C), C130(H13J,H13K,H13L),
 C34(H34A,H34B,H34C), C41(H41A,H41B,H41C), C61(H61A,H61B,H61C), C72(H72A,H72B,
 H72C), C27(H27A,H27B,H27C), C105(H10C,H10D,H10E), C35(H35A,H35B,H35C),
 C86(H86A,H86B,H86C), C38(H38A,H38B,H38C), C15(H15A,H15B,H15C), C82(H82A,H82B,
 H82C), C73(H73A,H73B,H73C), C106(H10F,H10G,H10H), C37(H37A,H37B,H37C),
 C129(H12P,H12Q,H12R), C16(H16A,H16B,H16C), C83(H83A,H83B,H83C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C36(H36A,H36B,H36C), C81(H81A,H81B,H81C)
;
_shelx_res_checksum              45967
_shelx_hkl_checksum              97358
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-07-06
_olex2_submission_original_sample_id hasj160706b
_olex2_submission_special_instructions 'No special instructions were received'