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_4088922
_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         'C38 H73 Ca K N4 Si4'
_chemical_formula_sum            'C38 H73 Ca K N4 Si4'
_chemical_formula_weight         777.54
_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             2016-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.4158(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9149(2)
_cell_length_b                   11.58948(14)
_cell_length_c                   21.6672(3)
_cell_measurement_reflns_used    9265
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.4220
_cell_measurement_theta_min      4.1130
_cell_volume                     4685.76(10)
_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      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 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega -114.00  -19.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -38.0000  120.0000 95

  2 omega  -68.00   28.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   57.0000  -90.0000 96

  3 omega  104.00  130.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000   60.0000 26

  4 omega   84.00  159.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   30.0000  -30.0000 75

  5 omega   27.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000   60.0000 82

  6 omega   91.00  176.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000   30.0000 85

  7 omega  142.00  176.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000   60.0000 34

  8 omega   32.00  125.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000   30.0000 93
;
_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      -0.0806638000
_diffrn_orient_matrix_UB_12      -0.0216891000
_diffrn_orient_matrix_UB_13      -0.0016836000
_diffrn_orient_matrix_UB_21      0.0048388000
_diffrn_orient_matrix_UB_22      0.0559265000
_diffrn_orient_matrix_UB_23      0.0650952000
_diffrn_orient_matrix_UB_31      -0.0170834000
_diffrn_orient_matrix_UB_32      0.1186642000
_diffrn_orient_matrix_UB_33      -0.0307891000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16064
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.116
_diffrn_reflns_theta_min         4.136
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.136
_exptl_absorpt_correction_T_max  0.912
_exptl_absorpt_correction_T_min  0.736
_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    1.102
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.3174
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.0604
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         8501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+0.5290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7568
_reflns_number_total             8501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00566_si_010.cif
_cod_data_source_block           hasj160404b
_cod_original_cell_volume        4685.75(10)
_cod_database_code               4088922
_chemical_oxdiff_formula         'C H N O Ca Si I K '
_reflns_odcompleteness_completeness 99.49
_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:
 C12(H12), C9(H9), C24(H24), C21(H21)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C5(H5), C19(H19), C17(H17), C18(H18)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C32(H32A,H32B,H32C), C27(H27A,H27B,H27C), C29(H29A,H29B,
 H29C), C35(H35A,H35B,H35C), C14(H14A,H14B,H14C), C28(H28A,H28B,H28C), C13(H13A,
 H13B,H13C), C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C),
 C37(H37A,H37B,H37C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C11(H11A,H11B,
 H11C), C10(H10A,H10B,H10C), C26(H26A,H26B,H26C), C34(H34A,H34B,H34C), C25(H25A,
 H25B,H25C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              30549
_shelx_hkl_checksum              58246
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-04-04
_olex2_submission_original_sample_id hasj160404b
_olex2_submission_special_instructions 'No special instructions were received'