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_7127739
_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         'C85 H116 N6 Ni2 P8 Si2'
_chemical_formula_sum            'C85 H116 N6 Ni2 P8 Si2'
_chemical_formula_weight         1643.19
_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   geom
_audit_creation_date             2020-06-11
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.05.22 svn.r1d9e7f8d for OlexSys, GUI svn.r6115)
;
_audit_update_record
;
2020-06-11 deposited with the CCDC.	2020-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.229(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.3638(5)
_cell_length_b                   16.0951(3)
_cell_length_c                   27.7549(6)
_cell_measurement_reflns_used    24504
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.9370
_cell_measurement_theta_min      4.2930
_cell_volume                     9968.7(4)
_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 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.963
_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     18.00 117.00   1.00   10.00    --   42.10  37.00-120.00   99
  2  \w     14.00 115.00   1.00   10.00    --   42.10  57.00 150.00  101
  3  \w     30.00  69.00   1.00   40.00    --  106.40 -30.00   0.00   39
  4  \w     24.00 109.00   1.00   40.00    --  106.40 -94.00 150.00   85
  5  \w     30.00  69.00   1.00   40.00    --  106.40 -30.00 -60.00   39
  6  \w     30.00  69.00   1.00   40.00    --  106.40 -30.00-120.00   39
  7  \w     30.00  69.00   1.00   40.00    --  106.40 -30.00 -30.00   39
  8  \w     33.00  77.00   1.00   40.00    --  106.40 -45.00 120.00   44
  9  \w     30.00  69.00   1.00   40.00    --  106.40 -30.00  30.00   39
 10  \w     30.00  69.00   1.00   40.00    --  106.40 -30.00 -90.00   39
 11  \w     34.00 135.00   1.00   40.00    --  106.40 -61.00-180.00  101
 12  \w     10.00 118.00   1.00   10.00    --   42.10  77.00 -30.00  108
 13  \w    -30.00  70.00   1.00   10.00    --   42.10 -57.00-150.00  100
 14  \w     78.00 158.00   1.00   40.00    --  106.40  30.00  60.00   80
 15  \w     81.00 136.00   1.00   40.00    --  106.40  45.00 -60.00   55
;
_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      0.0422633000
_diffrn_orient_matrix_UB_12      0.0141941000
_diffrn_orient_matrix_UB_13      0.0536344000
_diffrn_orient_matrix_UB_21      -0.0542465000
_diffrn_orient_matrix_UB_22      0.0008344000
_diffrn_orient_matrix_UB_23      0.0208205000
_diffrn_orient_matrix_UB_31      0.0058605000
_diffrn_orient_matrix_UB_32      -0.0946558000
_diffrn_orient_matrix_UB_33      0.0082140000
_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  0.0257
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            58661
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.102
_diffrn_reflns_theta_min         3.334
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.217
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.795
_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    1.095
_exptl_crystal_description       block
_exptl_crystal_F_000             3488
_exptl_crystal_recrystallization_method 'from n-hexane slow evaporation'
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1183
_refine_ls_number_reflns         19509
_refine_ls_number_restraints     654
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0582P)^2^+5.7654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1215
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16312
_reflns_number_total             19509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05365a2.cif
_cod_data_source_block           zic337_2
_cod_database_code               7127739
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C95 H140.5  N6 Ni2 P8 Si2 '
_chemical_oxdiff_usercomment     'from n-hexane slow evaporation'
_reflns_odcompleteness_completeness 99.18
_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. Uiso/Uaniso restraints and constraints
C02S \\sim C0AA \\sim C02D \\sim C1AA \\sim C02O \\sim C2AA \\sim C02A \\sim
C01Q \\sim C3AA \\sim C5 \\sim C01O \\sim C5AA \\sim C01U \\sim C6AA \\sim C01A
\\sim C7AA \\sim C021 \\sim C02B \\sim C9AA \\sim C02H \\sim C0 \\sim C0BA
\\sim C00K: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 1.7A
C02R \\sim C4AA \\sim C3 \\sim C3A \\sim C8AA \\sim C02T \\sim C1BA \\sim C02J
\\sim C2BA \\sim C3BA \\sim C02G \\sim C02K \\sim C5BA \\sim C4 \\sim C4A \\sim
C1 \\sim C029 \\sim C4BA \\sim C02Q \\sim C2 \\sim C02V \\sim C02U \\sim C02L:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C02M \\sim C16 \\sim C026 \\sim C26 \\sim C02E \\sim C28 \\sim C027 \\sim C29
\\sim C02I \\sim C48: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
3. Others
 Sof(C1BA)=Sof(C2BA)=Sof(H2BA)=Sof(C3BA)=Sof(H3BA)=Sof(C5BA)=Sof(H5BA)=
 Sof(C4A)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(C1AA)=Sof(H1AA)=Sof(C2AA)=
 Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C0)=Sof(H0)=Sof(C9AA)=Sof(H9AA)=Sof(H9AB)=
 Sof(H9AC)=Sof(C0BA)=Sof(H0BA)=Sof(H0BB)=Sof(H0BC)=Sof(C4AA)=Sof(H4AA)=
 Sof(C8AA)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=
 Sof(C02V)=Sof(H19)=Sof(HW)=Sof(HX)=Sof(C2)=Sof(H2A)=Sof(C4BA)=Sof(H4BA)=
 Sof(H4BB)=Sof(H4BC)=Sof(C5)=Sof(H5A)=Sof(C5AA)=Sof(H5AA)=Sof(C6AA)=Sof(H6AA)=
 Sof(C7AA)=Sof(C3AA)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C26)=Sof(C28)=Sof(H28)=
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C48)=1-FVAR(1)
 Sof(C01A)=Sof(C01Q)=Sof(C01U)=Sof(H6)=Sof(C021)=Sof(H021)=Sof(C026)=Sof(C027)=
 Sof(C029)=Sof(H029)=Sof(C02A)=Sof(H02G)=Sof(C02B)=Sof(H02H)=Sof(H02I)=
 Sof(H02J)=Sof(C02D)=Sof(H02N)=Sof(C02E)=Sof(H02O)=Sof(C02G)=Sof(H02S)=
 Sof(C02H)=Sof(H02T)=Sof(H02U)=Sof(H02V)=Sof(C02I)=Sof(H02W)=Sof(H02X)=
 Sof(C02J)=Sof(C02K)=Sof(H02Y)=Sof(C02L)=Sof(H02Z)=Sof(C02M)=Sof(H02)=Sof(HG)=
 Sof(HH)=Sof(C02O)=Sof(H11)=Sof(HK)=Sof(HL)=Sof(C02Q)=Sof(H13)=Sof(HO)=Sof(HP)=
 Sof(C02R)=Sof(H14)=Sof(C02S)=Sof(H15)=Sof(HQ)=Sof(HR)=Sof(C02T)=Sof(H16)=
 Sof(HS)=Sof(HT)=Sof(C02U)=Sof(H17)=Sof(HU)=Sof(HV)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(H3C)=Sof(C01O)=Sof(H18)=Sof(C4)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C00R(H00R), C00X(H00X), C011(H011), C012(H012), C013(H013), C019(H019),
 C01S(H4), C021(H021), C023(H023), C029(H029), C02D(H02N), C02R(H14),
 C1AA(H1AA), C0(H0), C4AA(H4AA), C2(H2A)
4.b Aromatic/amide H refined with riding coordinates:
 C00L(H00L), C00T(H00T), C00U(H00U), C00V(H00V), C00Y(H00Y), C015(H015),
 C01L(H01Z), C01N(H1), C01P(H2), C01U(H6), C01V(H7), C2BA(H2BA), C3BA(H3BA),
 C5BA(H5BA), C01Y(H8), C01Z(H9), C020(H020), C022(H022), C028(H028), C02A(H02G),
  C02E(H02O), C02G(H02S), C02K(H02Y), C02L(H02Z), C01O(H18), C5(H5A),
 C5AA(H5AA), C6AA(H6AA), C28(H28)
4.c Fitted hexagon refined as free rotating group:
 C1BA(C2BA,C3BA,C5BA,C4A,C1), C5(C5AA,C6AA,C7AA,C00K,C3AA)
4.d X=CH2 refined with riding coordinates:
 C017(H01A,H01B), C02I(H02W,H02X), C16(H16A,H16B)
4.e Idealised Me refined as rotating group:
 C01B(H01C,H01D,H01E), C01C(H01F,H01G,H01H), C01D(H01I,H01J,H01K), C01E(H01L,
 H01M,H01N), C01F(H01O,H01P,H01Q), C01G(H01R,H01S,H01T), C01J(H01U,H01V,H01W),
 C01K(H01X,H01Y,H), C01M(H01,HA,HB), C01R(H3,HC,HD), C01T(H5,HE,HF), C024(H02A,
 H02B,H02C), C025(H02D,H02E,H02F), C02B(H02H,H02I,H02J), C02C(H02K,H02L,H02M),
 C02F(H02P,H02Q,H02R), C02H(H02T,H02U,H02V), C02M(H02,HG,HH), C02N(H10,HI,HJ),
 C02O(H11,HK,HL), C02P(H12,HM,HN), C02Q(H13,HO,HP), C02S(H15,HQ,HR), C02T(H16,
 HS,HT), C02U(H17,HU,HV), C3(H3A,H3B,H3C), C0AA(H0AA,H0AB,H0AC), C2AA(H2AA,H2AB,
 H2AC), C9AA(H9AA,H9AB,H9AC), C0BA(H0BA,H0BB,H0BC), C8AA(H8AA,H8AB,H8AC),
 C3A(H3AA,H3AB,H3AC), C02V(H19,HW,HX), C4BA(H4BA,H4BB,H4BC), C29(H29A,H29B,H29C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.203
_oxdiff_exptl_absorpt_empirical_full_min 0.776