Understanding the Solution and Solid-State Structures of Pd and Pt PSiP Pincer-Supported Hydrides.
Suh, Hee-Won; Balcells, David; Edwards, Alison J.; Guard, Louise M.; Hazari, Nilay; Mader, Elizabeth A.; Mercado, Brandon Q.; Repisky, Michal; Inorganic chemistry 54 (2015) 11411–11422; doi:10.1021/acs.inorgchem.5b02073

data_4344446
_publ_section_title
;
 Understanding the Solution and Solid-State Structures of Pd and Pt PSiP
 Pincer-Supported Hydrides.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11411
_journal_page_last               11422
_journal_paper_doi               10.1021/acs.inorgchem.5b02073
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C37 H56 P2 Pd Si, 1.5(C5 H12)'
_chemical_formula_sum            'C44.5 H74 P2 Pd Si'
_chemical_formula_weight         805.46
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
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_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
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CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
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CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
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;
_diffrn_measurement_device
;
AFC11 (Left): Eulerian 3 circle
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_diffrn_measurement_device_type  'Rigaku Saturn944+ (2x2 bin mode)'
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_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.030711
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_diffrn_orient_matrix_UB_13      -0.009922
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_diffrn_orient_matrix_UB_31      0.010536
_diffrn_orient_matrix_UB_32      -0.009919
_diffrn_orient_matrix_UB_33      0.040863
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0855
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_laue_measured_fraction_full 0.903
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_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            204543
_diffrn_reflns_point_group_measured_fraction_full 0.903
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_diffrn_source                   'Rotating Anode'
_diffrn_source_current           40.0
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_exptl_crystal_colour            Colorless
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_exptl_crystal_description       block
_exptl_crystal_F_000             3448
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_refine_diff_density_max         1.361
_refine_diff_density_min         -0.787
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_refine_ls_extinction_method     none
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+10.4627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_cod_data_source_file            ic5b02073_si_002.cif
_cod_data_source_block           '_(CyPSiP)PdH'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4344446--4344451.cif.
;
_cod_database_code               4344446
_shelxl_version_number           2013-4
_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. Restrained distances
 C86-C85 \\sim C86-C87 \\sim C88-C87 \\sim C89-C88
 with sigma of 0.02
 C76-C75 \\sim C77-C76 \\sim C77-C78 \\sim C78-C79
 with sigma of 0.02
 C83-C84 \\sim C82-C83 \\sim C81-C82 \\sim C81-C80
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C85, C86, C87, C88, C89
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C78, C79, C77, C76, C75
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C84, C83, C82, C81, C80
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C32(H32), C7(H7), C44(H44), C63(H63), C69(H69), C38(H38), C31(H31), C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C37(H37A,H37B), C33(H33A,H33B), C42(H42A,H42B), C8(H8A,H8B),
 C48(H48A,H48B), C12(H12A,H12B), C68(H68A,H68B), C10(H10A,H10B), C40(H40A,H40B),
  C49(H49A,H49B), C11(H11A,H11B), C35(H35A,H35B), C39(H39A,H39B), C36(H36A,
 H36B), C43(H43A,H43B), C9(H9A,H9B), C70(H70A,H70B), C45(H45A,H45B), C34(H34A,
 H34B), C41(H41A,H41B), C71(H71A,H71B), C30(H30A,H30B), C74(H74A,H74B),
 C73(H73A,H73B), C67(H67A,H67B), C65(H65A,H65B), C66(H66A,H66B), C72(H72A,H72B),
  C2(H2A,H2B), C64(H64A,H64B), C26(H26A,H26B), C29(H29A,H29B), C28(H28A,H28B),
 C5(H5A,H5B), C3(H3A,H3B), C4(H4A,H4B), C27(H27A,H27B), C47(H47A,H47B), C6(H6A,
 H6B), C87(H87A,H87B), C86(H86A,H86B), C88(H88A,H88B), C83(H83A,H83B), C82(H82A,
 H82B), C81(H81A,H81B), C78(H78A,H78B), C76(H76A,H76B), C77(H77A,H77B)
4.c Me refined as rotating group:
 C80(H80A,H80B,H80C), C84(H84A,H84B,H84C)
4.d Aromatic/amide H refined with riding coordinates:
 C58(H58), C17(H17), C24(H24), C21(H21), C15(H15), C51(H51), C54(H54),
 C14(H14), C52(H52), C53(H53), C61(H61), C16(H16), C59(H59), C23(H23), C22(H22),
  C60(H60)
4.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C56(H56A,H56B,H56C), C85(H85A,H85B,H85C), C89(H89A,H89B,
 H89C), C79(H79A,H79B,H79C), C75(H75A,H75B,H75C)
;
_shelx_res_checksum              62764
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