β-Diketiminate calcium hydride complexes: the importance of solvent effects.
Causero, Andrea; Ballmann, Gerd; Pahl, Jürgen; Färber, Christian; Intemann, Julia; Harder, Sjoerd; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1822–1831; doi:10.1039/c6dt04659b

data_7041821
_publ_section_title
;
 \b-Diketiminate calcium hydride complexes: the importance of solvent
 effects.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1822
_journal_page_last               1831
_journal_paper_doi               10.1039/c6dt04659b
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C40 H70 Ca N4 O Si2'
_chemical_formula_sum            'C40 H70 Ca N4 O Si2'
_chemical_formula_weight         719.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2016-11-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.24 svn.r3356 for OlexSys, GUI svn.r5267)
;
_audit_update_record
;
2016-12-02 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                102.3440(10)
_cell_angle_beta                 90.1900(10)
_cell_angle_gamma                90.3460(10)
_cell_formula_units_Z            8
_cell_length_a                   11.30050(10)
_cell_length_b                   20.2024(2)
_cell_length_c                   39.1907(2)
_cell_measurement_reflns_used    44642
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.6970
_cell_measurement_theta_min      3.4390
_cell_volume                     8740.03(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 10.5806
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.9947
_diffrn_measured_fraction_theta_max 0.9947
_diffrn_measurement_details
;
  1 omega -128.00   45.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909    0.0000  -30.0000 346

  2 omega -114.00  -19.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -38.0000  120.0000 190

  3 omega  -96.00   -2.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  125.0000 -180.0000 188

  4 omega   23.00   97.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909 -125.0000  120.0000 148

  5 omega    1.00   82.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909  -99.0000    0.0000 162

  6 omega   31.00  130.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000 -150.0000 198

  7 omega   25.00  109.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000 -180.0000 168

  8 omega   26.00  151.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -15.0000  -30.0000 250

  9 omega   32.00  137.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000  -30.0000 210

 10 omega   25.00  109.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000  -90.0000 168

 11 omega   31.00  130.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  120.0000 198

 12 omega   82.00  177.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000  150.0000 190

 13 omega   34.00  121.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000  150.0000 174

 14 omega -112.00  -15.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000 -120.0000 194

 15 omega -116.00  -10.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -77.0000   90.0000 212

 16 omega -116.00  -10.00   0.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -77.0000    0.0000 212

 17 omega   61.00  178.00   0.5000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   15.0000   30.0000 234
;
_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      -0.1100421000
_diffrn_orient_matrix_UB_12      -0.0463356000
_diffrn_orient_matrix_UB_13      -0.0072661000
_diffrn_orient_matrix_UB_21      -0.0720463000
_diffrn_orient_matrix_UB_22      0.0528189000
_diffrn_orient_matrix_UB_23      0.0257158000
_diffrn_orient_matrix_UB_31      -0.0358645000
_diffrn_orient_matrix_UB_32      0.0340147000
_diffrn_orient_matrix_UB_33      -0.0300858000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            86599
_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         3.463
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.003
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.963
_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    1.093
_exptl_crystal_description       block
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.3013
_exptl_crystal_size_mid          0.2119
_exptl_crystal_size_min          0.171
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1805
_refine_ls_number_reflns         31761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.003
_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^+2.2710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28862
_reflns_number_total             31761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04659b2.cif
_cod_data_source_block           hasj161128a
_cod_depositor_comments
;
Adding full bibliography for 7041815--7041821.cif.

2017-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '4(C40 H70 Ca N4 O Si2)'
_cod_original_formula_sum        'C160 H280 Ca4 N16 O4 Si8'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     2877.02
_cod_database_code               7041821
_chemical_oxdiff_formula         'C H N Ca Si O'
_reflns_odcompleteness_completeness 99.47
_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:
 C64(H64), C15(H15), C92(H92), C24(H24), C12(H12), C107(H107), C144(H144),
 C135(H135), C55(H55), C27(H27), C52(H52), C147(H147), C95(H95), C132(H132),
 C67(H67), C104(H104)
2.b Secondary CH2 refined with riding coordinates:
 C78(H78A,H78B), C156(H15A,H15B), C76(H76A,H76B), C79(H79A,H79B), C38(H38A,
 H38B), C157(H15F,H15G), C159(H15N,H15O), C118(H11A,H11B), C119(H11C,H11D),
 C77(H77A,H77B), C36(H36A,H36B), C158(H15P,H15Q), C39(H39A,H39B), C37(H37A,
 H37B), C117(H11K,H11L), C116(H11M,H11N)
2.c Aromatic/amide H refined with riding coordinates:
 C122(H122), C90(H90), C9(H9), C8(H8), C88(H88), C140(H140), C89(H89),
 C10(H10), C42(H42), C62(H62), C20(H20), C48(H48), C49(H49), C22(H22), C60(H60),
  C141(H141), C100(H100), C142(H142), C130(H130), C61(H61), C102(H102),
 C129(H129), C101(H101), C21(H21), C50(H50), C128(H128)
2.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C84(H84A,H84B,H84C), C45(H45A,H45B,H45C), C44(H44A,H44B,
 H44C), C125(H12D,H12E,H12F), C124(H12G,H12H,H12I), C154(H15C,H15D,H15E),
 C75(H75A,H75B,H75C), C155(H15H,H15I,H15J), C150(H15K,H15L,H15M), C72(H72A,H72B,
 H72C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C), C16(H16A,H16B,H16C),
 C114(H11E,H11F,H11G), C5(H5A,H5B,H5C), C35(H35A,H35B,H35C), C146(H14D,H14E,
 H14F), C85(H85A,H85B,H85C), C112(H11H,H11I,H11J), C93(H93A,H93B,H93C),
 C109(H10A,H10B,H10C), C73(H73A,H73B,H73C), C71(H71A,H71B,H71C), C17(H17A,H17B,
 H17C), C74(H74A,H74B,H74C), C32(H32A,H32B,H32C), C65(H65A,H65B,H65C), C53(H53A,
 H53B,H53C), C31(H31A,H31B,H31C), C115(H11O,H11P,H11Q), C80(H80A,H80B,H80C),
 C136(H13D,H13E,H13F), C111(H11R,H11S,H11T), C28(H28A,H28B,H28C), C160(H16D,
 H16E,H16F), C94(H94A,H94B,H94C), C66(H66A,H66B,H66C), C54(H54A,H54B,H54C),
 C96(H96A,H96B,H96C), C152(H15R,H15S,H15T), C153(H15U,H15V,H15W), C13(H13A,H13B,
 H13C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C113(H11U,H11V,H11W),
 C110(H11X,H11Y,H), C14(H14A,H14B,H14C), C137(H13G,H13H,H13I), C151(H15X,H15Y,
 HA), C145(H14G,H14H,H14I), C149(H14J,H14K,H14L), C25(H25A,H25B,H25C), C57(H57A,
 H57B,H57C), C120(H12A,H12B,H12C), C70(H70A,H70B,H70C), C97(H97A,H97B,H97C),
 C56(H56A,H56B,H56C), C148(H14M,H14N,H14O), C106(H10D,H10E,H10F), C108(H10G,
 H10H,H10I), C105(H10J,H10K,H10L), C40(H40A,H40B,H40C), C26(H26A,H26B,H26C),
 C69(H69A,H69B,H69C), C134(H13J,H13K,H13L), C68(H68A,H68B,H68C), C133(H13M,H13N,
 H13O)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-11-28
_olex2_submission_original_sample_id hasj161128a
_olex2_submission_special_instructions 'No special instructions were received'