An unusual Ni<sub>2</sub>Si<sub>2</sub>P<sub>8</sub> cluster formed by complexation and thermolysis.
Ziegler, Christoph G. P.; Taube, Clemens; Kelly, John A.; Hierlmeier, Gabriele; Uttendorfer, Maria; Weigand, Jan J.; Wolf, Robert; Chemical communications (Cambridge, England) 56 (2020) 14071–14074; doi:10.1039/d0cc05365a

data_7127737
_publ_section_title
;
 An unusual Ni<sub>2</sub>Si<sub>2</sub>P<sub>8</sub> cluster formed by
 complexation and thermolysis.
;
_journal_issue                   90
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              14071
_journal_page_last               14074
_journal_paper_doi               10.1039/d0cc05365a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C79 H104 N6 Ni P8 Si2, C6 H14'
_chemical_formula_sum            'C85 H118 N6 Ni P8 Si2'
_chemical_formula_weight         1586.50
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-29
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.05.22 svn.r3605 for OlexSys, GUI svn.r5790)
;
_audit_update_record
;
2020-06-11 deposited with the CCDC.	2020-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.889(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4813(3)
_cell_length_b                   22.9979(3)
_cell_length_c                   22.0196(3)
_cell_measurement_reflns_used    16410
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      72.7620
_cell_measurement_theta_min      3.9080
_cell_volume                     8768.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.18b (Rigaku OD, 2018)'
_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      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -42.00  30.00   1.00   17.50    --  -42.68  37.00 -30.00   72
  2  \w    -26.00  36.00   1.00   17.50    --  -42.68  19.00  30.00   62
  3  \w    -26.00  36.00   1.00   17.50    --  -42.68  19.00 -90.00   62
  4  \w     80.00 158.00   1.00   45.00    --  104.13  45.00 -60.00   78
  5  \w     77.00 158.00   1.00   45.00    --  104.13  61.00 120.00   81
  6  \w     23.00 109.00   1.00   45.00    --  104.13 -94.00-120.00   86
  7  \w     80.00 158.00   1.00   45.00    --  104.13  45.00  90.00   78
  8  \w     77.00 158.00   1.00   45.00    --  104.13  61.00   0.00   81
  9  \w     34.00  71.00   1.00   45.00    --  104.13 -61.00 -60.00   37
 10  \w      2.00  57.00   1.00   17.50    --   42.68-125.00 150.00   55
 11  \w     11.00 117.00   1.00   17.50    --   42.68  77.00-120.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0699805000
_diffrn_orient_matrix_UB_12      -0.0388165000
_diffrn_orient_matrix_UB_13      0.0227197000
_diffrn_orient_matrix_UB_21      0.0533400000
_diffrn_orient_matrix_UB_22      0.0424168000
_diffrn_orient_matrix_UB_23      -0.0283353000
_diffrn_orient_matrix_UB_31      0.0127893000
_diffrn_orient_matrix_UB_32      0.0344046000
_diffrn_orient_matrix_UB_33      0.0605903000
_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  0.0293
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41046
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.110
_diffrn_reflns_theta_min         3.591
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.303
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.463
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.18b (Rigaku Oxford Diffraction, 2018)
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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       needle
_exptl_crystal_F_000             3384
_exptl_crystal_recrystallization_method 'from n-hexane'
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     984
_refine_ls_number_reflns         16774
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0453P)^2^+6.2845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13805
_reflns_number_total             16774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05365a2.cif
_cod_data_source_block           zic223_mp
_cod_database_code               7127737
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C316 H416 N24 Ni4 P32 Si8 '
_chemical_oxdiff_usercomment     'from n-hexane'
_reflns_odcompleteness_completeness 98.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 C83-C84 \\sim C84-C85 \\sim C85-C86 \\sim C86-C87 \\sim C87-C82
 with sigma of 0.02
 C83-C85 \\sim C85-C87 \\sim C84-C86 \\sim C86-C82
 with sigma of 0.04
 C81-C88 \\sim C88-C32 \\sim C32-C89 \\sim C89-C90 \\sim C90-C91
 with sigma of 0.02
 C81-C32 \\sim C32-C90 \\sim C88-C89 \\sim C89-C91
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C82: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C81 \\sim C88 \\sim C32 \\sim C89 \\sim C90 \\sim C91: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C83, C84, C85, C86, C87, C82
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C81, C88, C32, C89, C90, C91
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C83(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C84(0.5) H3A(0.5) H3B(0.5)
 C85(0.5) H4A(0.5) H4B(0.5) C86(0.5) H5A(0.5) H5B(0.5) C87(0.5) H6A(0.5)
 H6B(0.5) C82(0.5) H7A(0.5) H7B(0.5) H7C(0.5) C81(0.5) H1A(0.5) H1B(0.5)
 H1C(0.5) C88(0.5) H8A(0.5) H8B(0.5) C32(0.5) H9A(0.5) H9B(0.5) C89(0.5)
 H10A(0.5) H10B(0.5) C90(0.5) H11A(0.5) H11B(0.5) C91(0.5) H12A(0.5) H12B(0.5)
 H12C(0.5)
6.a Free rotating group:
 C83(C84,C85,C86,C87,C82), C81(C88,C32,C89,C90,C91)
6.b Ternary CH refined with riding coordinates:
 C27(H00X), C45(H017), C54(H018), C16(H01D), C42(H01O), C57(H020), C12(H022),
 C24(H02W)
6.c Secondary CH2 refined with riding coordinates:
 C84(H3A,H3B), C85(H4A,H4B), C86(H5A,H5B), C87(H6A,H6B), C88(H8A,H8B), C32(H9A,
 H9B), C89(H10A,H10B), C90(H11A,H11B)
6.d Me refined with riding coordinates:
 C83(H2A,H2B,H2C)
6.e Aromatic/amide H refined with riding coordinates:
 C33(H00O), C61(H00S), C60(H015), C65(H016), C20(H01G), C67(H01H), C3(H01L),
 C50(H01M), C22(H01N), C75(H01S), C52(H01T), C21(H01Z), C10(H01), C8(H1),
 C74(H15), C38(H3), C9(H4), C51(H5), C39(H027), C40(H02S)
6.f X=CH2 refined with riding coordinates:
 C1(H6,HF)
6.g Idealised Me refined as rotating group:
 C35(H00A,H00B,H00C), C69(H01A,H01B,H2), C71(H01I,H01J,H01K), C80(H01P,H01Q,
 H01R), C29(H01U,H01V,H01W), C55(H01X,H01Y,H), C58(H02A,H02B,H02C), C15(H02D,
 H02E,H02F), C46(H02G,H02H,H02I), C28(H02J,H02K,H02L), C44(H02M,H02N,H02O),
 C26(H02P,H02Q,H02R), C78(H02T,H02U,H02V), C47(H02X,H02Y,HA), C5(H02Z,HB,HC),
 C56(H02,HD,HE), C70(H7,HG,HH), C59(H8,HI,HJ), C43(H9,HK,HL), C13(H10,HM,HN),
 C14(H11,HO,HP), C17(H12,HQ,HR), C25(H13,HS,HT), C77(H14,HU,HV), C82(H7A,H7B,
 H7C), C81(H1A,H1B,H1C), C91(H12A,H12B,H12C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              40195
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.231
_oxdiff_exptl_absorpt_empirical_full_min 0.870