Co-crystal of Ti4Ni2 and Ti8Ni4 clusters with enhanced photochemical properties
Wang, Chao; Lu, Yong Jun; Rao, Ming Yang; Chen, Ning; Wang, Shou Juan; Kong, Fan Gong; CrystEngComm 23 (2021) 4402–4407; doi:10.1039/D1CE00369K

data_7242885
_publ_section_title
;
 Co-crystal of Ti4Ni2 and Ti8Ni4 clusters with enhanced photochemical
 properties
;
_journal_issue                   24
_journal_name_full               CrystEngComm
_journal_page_first              4402
_journal_page_last               4407
_journal_paper_doi               10.1039/D1CE00369K
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety
'C136 H114 N2 Ni4 O50 Ti8, C80 H64 Ni2 O28 Ti4, 5(C2 H3 N)'
_chemical_formula_sum            'C226 H193 N7 Ni6 O78 Ti12'
_chemical_formula_weight         5181.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-12-27 deposited with the CCDC.	2021-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                78.5920(10)
_cell_angle_beta                 79.3250(10)
_cell_angle_gamma                71.8550(10)
_cell_formula_units_Z            1
_cell_length_a                   13.2237(2)
_cell_length_b                   15.5692(2)
_cell_length_c                   30.2206(4)
_cell_measurement_reflns_used    38411
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.8940
_cell_measurement_theta_min      3.0050
_cell_volume                     5744.39(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.960
_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    -73.00  -7.00   0.50    2.00    --  -43.30 106.00 -85.00  132
  2  \w    -51.00 -10.00   0.50    2.00    --  -43.30 125.00   0.00   82
  3  \w    -54.00 -28.00   0.50    2.50    --  -90.25 106.00 -85.00   52
  4  \w    -53.00 -27.00   0.50    2.50    --  -90.25 125.00 -30.00   52
  5  \w    -65.00  24.00   0.50    2.00    --  -43.30  57.00 -60.00  178
  6  \w    -63.00  30.00   0.50    2.00    --  -43.30  37.00  60.00  186
  7  \w     16.00  87.00   0.50    2.00    --   43.30-106.00 175.00  142
  8  \w     61.00 112.00   0.50    2.50    --  109.88-106.00 175.00  102
  9  \w     87.00 137.00   0.50    2.50    --  109.88 -77.00 120.00  100
 10  \w    107.00 134.00   0.50    2.50    --  109.88 -30.00   0.00   54
 11  \w    137.00 167.00   0.50    2.50    --  109.88  30.00 -30.00   60
 12  \w    102.00 145.00   0.50    2.50    --  109.88 106.00 -85.00   86
 13  \w     99.00 174.00   0.50    2.50    --  109.88  45.00-120.00  150
 14  \w     86.00 120.00   0.50    2.50    --  109.88  30.00 -30.00   68
 15  \w     74.00 132.00   0.50    2.50    --  109.88 -45.00 -90.00  116
 16  \w     76.00 128.00   0.50    2.50    --  109.88  15.00-120.00  104
 17  \w     69.00 107.00   0.50    2.50    --  109.88 -94.00-150.00   76
 18  \w     41.00  66.00   0.50    2.50    --  109.88 -45.00 -90.00   50
 19  \w     36.00 108.00   0.50    2.50    --  109.88 -94.00 -90.00  144
 20  \w     62.00  88.00   0.50    2.50    --  109.88 -94.00   0.00   52
 21  \w     62.00 108.00   0.50    2.50    --  109.88 -94.00  30.00   92
 22  \w     55.00 108.00   0.50    2.50    --  109.88 -94.00 -30.00  106
 23  \w     31.00 128.00   0.50    2.50    --  109.88 -30.00 120.00  194
 24  \w     43.00  70.00   0.50    2.50    --  109.88 -77.00 120.00   54
 25  \w     37.00  94.00   0.50    2.50    --  109.88 -94.00 120.00  114
 26  \w     32.00 101.00   0.50    2.50    --  109.88 -30.00   0.00  138
 27  \w     34.00 132.00   0.50    2.50    --  109.88 -45.00-120.00  196
 28  \w     36.00  86.00   0.50    2.50    --  109.88 -94.00  60.00  100
 29  \w   -111.00 -80.00   0.50    2.00    --  -43.30-125.00-120.00   62
 30  \w   -106.00 -71.00   0.50    2.00    --  -43.30-125.00-150.00   70
 31  \w   -124.00 -99.00   0.50    2.50    --  -90.25 -94.00 -60.00   50
 32  \w   -156.00-127.00   0.50    2.50    --  -90.25 -94.00 -60.00   58
 33  \w   -160.00-114.00   0.50    2.50    --  -90.25 -30.00 -60.00   92
 34  \w   -103.00 -69.00   0.50    2.50    --  -90.25 -30.00 -60.00   68
 35  \w   -131.00-105.00   0.50    2.50    --  -90.25 -94.00  30.00   52
 36  \w   -111.00 -20.00   0.50    2.00    --  -43.30 -57.00 150.00  182
 37  \w   -119.00 -94.00   0.50    2.50    --  -90.25-106.00 175.00   50
 38  \w   -163.00-129.00   0.50    2.50    --  -90.25 -45.00  60.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0758190000
_diffrn_orient_matrix_UB_12      0.0187945000
_diffrn_orient_matrix_UB_13      -0.0360465000
_diffrn_orient_matrix_UB_21      0.0798515000
_diffrn_orient_matrix_UB_22      0.0390428000
_diffrn_orient_matrix_UB_23      -0.0358421000
_diffrn_orient_matrix_UB_31      0.0563441000
_diffrn_orient_matrix_UB_32      -0.0959927000
_diffrn_orient_matrix_UB_33      -0.0129988000
_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  0.0240
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            66541
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.200
_diffrn_reflns_theta_min         3.010
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.608
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       block
_exptl_crystal_F_000             2654
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1505
_refine_ls_number_reflns         23107
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0672P)^2^+7.2160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21251
_reflns_number_total             23107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00369k2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7242884--7242885.cif.'
_cod_original_cell_volume        5744.40(14)
_cod_database_code               7242885
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'c n h  o ni'
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N4) \\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C114) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 N4, C113, C114
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: N4(0.5) C113(0.5) C114(0.5) H11D(0.5) H11E(0.5) H11F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C18(H18), C29(H29), C30(H30), C33(H33), C34(H34), C36(H36),
 C38(H38), C40(H40), C41(H41), C46(H46), C47(H47), C50(H50), C53(H53), C54(H54),
  C56(H56), C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64),
 C65(H65), C67(H67), C68(H68), C69(H69), C71(H71), C73(H73), C74(H74), C79(H79),
  C81(H81), C83(H83), C86(H86), C87(H87), C88(H88), C90(H90), C92(H92),
 C98(H98), C99(H99), C101(H101), C102(H102), C105(H105), C35(H35), C39(H39),
 C42(H42), C49(H49), C52(H52), C57(H57), C66(H66), C72(H72), C75(H75), C76(H76),
  C77(H77), C80(H80), C84(H84), C89(H89), C91(H91), C93(H93), C94(H94),
 C95(H95), C97(H97), C100(H100), C103(H103), C104(H104), C106(H106), C108(H108),
  C109(H109), C112(H112)
5.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C43(H43A,H43B,H43C), C55(H55A,H55B,H55C), C82(H82A,H82B,
 H82C), C107(H10A,H10B,H10C), C70(H70A,H70B,H70C), C85(H85A,H85B,H85C),
 C96(H96A,H96B,H96C), C111(H11A,H11B,H11C), C114(H11D,H11E,H11F)
;
_shelx_res_checksum              96251
_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 2.059
_oxdiff_exptl_absorpt_empirical_full_min 0.804