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_4088930
_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         'C113 H166 Ca3 N6 O2, C6 H14'
_chemical_formula_sum            'C119 H180 Ca3 N6 O2'
_chemical_formula_weight         1846.92
_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   mixed
_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                92.8035(13)
_cell_angle_beta                 101.6317(12)
_cell_angle_gamma                114.0730(15)
_cell_formula_units_Z            2
_cell_length_a                   15.1967(2)
_cell_length_b                   18.2301(3)
_cell_length_c                   25.8609(4)
_cell_measurement_reflns_used    18715
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.5530
_cell_measurement_theta_min      3.2080
_cell_volume                     6337.71(19)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega  -50.00   31.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   38.0000  -30.0000 81

  2 omega  -67.00   28.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   57.0000 -180.0000 95

  3 omega   46.00   97.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909 -125.0000    0.0000 51

  4 omega   35.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000  120.0000 86

  5 omega   31.00   88.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  -60.0000 57

  6 omega   63.00  137.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000  -90.0000 74

  7 omega  108.00  134.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -61.0000 -150.0000 26

  8 omega   82.00  178.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   30.0000  -30.0000 96

  9 omega   94.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000 -120.0000 83

 10 omega   89.00  174.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000   60.0000 85

 11 omega   40.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -61.0000 -150.0000 57

 12 omega   25.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000 -180.0000 84

 13 omega   31.00   90.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  150.0000 59

 14 omega -112.00  -18.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000   30.0000 94
;
_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      -0.0019010000
_diffrn_orient_matrix_UB_12      0.0473905000
_diffrn_orient_matrix_UB_13      -0.0476114000
_diffrn_orient_matrix_UB_21      0.0452508000
_diffrn_orient_matrix_UB_22      -0.0478459000
_diffrn_orient_matrix_UB_23      -0.0276919000
_diffrn_orient_matrix_UB_31      -0.1051199000
_diffrn_orient_matrix_UB_32      -0.0649605000
_diffrn_orient_matrix_UB_33      -0.0273258000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            39256
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.118
_diffrn_reflns_theta_min         3.234
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.463
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.920
_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    0.968
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.3117
_exptl_crystal_size_mid          0.2182
_exptl_crystal_size_min          0.1941
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1209
_refine_ls_number_reflns         22879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0552
_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^)+(0.1050P)^2^+0.6140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1623
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19188
_reflns_number_total             22879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00566_si_006.cif
_cod_data_source_block           hasj151127b
_cod_original_cell_volume        6337.72(18)
_cod_database_code               4088930
_chemical_oxdiff_formula         'C H N Ca O Si K'
_reflns_odcompleteness_completeness 99.08
_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:
 C53(H53), C21(H21), C8(H8), C18(H18), C30(H30), C65(H65), C68(H68), C33(H33),
 C56(H56), C100(H100), C41(H41), C45(H45), C6(H6), C43(H43), C78(H78),
 C103(H103), C10(H10), C80(H80), C88(H88), C76(H76), C91(H91)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C39(H39A,H39B), C40(H40A,H40B), C9(H9A,H9B), C4(H4A,H4B),
 C79(H79A,H79B), C7(H7A,H7B), C5(H5A,H5B), C113(H11A,H11B), C108(H10D,H10E),
 C38(H38A,H38B), C46(H46A,H46B), C106(H10F,H10G), C112(H11C,H11D), C109(H10H,
 H10I), C44(H44A,H44B), C107(H10J,H10K), C74(H74A,H74B), C111(H11E,H11F),
 C42(H42A,H42B), C11(H11G,H11H), C77(H77A,H77B), C73(H73A,H73B), C110(H11I,
 H11J), C75(H75A,H75B), C81(H81A,H81B), C118(H11N,H11O), C117(H11P,H11Q),
 C115(H11U,H11V), C116(H11W,H11X)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C14(H14), C49(H49), C28(H28), C61(H61), C15(H15), C85(H85),
 C26(H26), C84(H84), C27(H27), C62(H62), C63(H63), C86(H86), C51(H51), C50(H50),
  C98(H98), C96(H96), C97(H97)
2.d Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C32(H32A,H32B,H32C), C101(H10A,H10B,H10C), C34(H34A,H34B,
 H34C), C23(H23A,H23B,H23C), C67(H67A,H67B,H67C), C70(H70A,H70B,H70C), C20(H20A,
 H20B,H20C), C57(H57A,H57B,H57C), C54(H54A,H54B,H54C), C66(H66A,H66B,H66C),
 C19(H19A,H19B,H19C), C31(H31A,H31B,H31C), C58(H58A,H58B,H58C), C22(H22A,H22B,
 H22C), C35(H35A,H35B,H35C), C105(H10L,H10M,H10N), C90(H90A,H90B,H90C),
 C102(H10O,H10P,H10Q), C89(H89A,H89B,H89C), C69(H69A,H69B,H69C), C93(H93A,H93B,
 H93C), C104(H10R,H10S,H10T), C92(H92A,H92B,H92C), C114(H11K,H11L,H11M),
 C119(H11R,H11S,H11T)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-11-27
_olex2_submission_original_sample_id hasj151127b
_olex2_submission_special_instructions 'No special instructions were received'