Structural diversity and photocatalytic activity of six Co(ii)/Ni(ii) complexes with three flexible phenylenediacetate isomers
Zhang, Mei-Li; Bai, Ye; Ren, Yi-Xia; Wang, Ji-Jiang; Yang, Xiao-Gang; Ma, Lu-Fang; CrystEngComm 23 (2021) 1616–1627; doi:10.1039/D0CE01702G

data_7242114
_publ_section_title
;
 Structural diversity and photocatalytic activity of six Co(ii)/Ni(ii)
 complexes with three flexible phenylenediacetate isomers
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1616
_journal_page_last               1627
_journal_paper_doi               10.1039/D0CE01702G
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C78 H72 N16 Ni3 O16, 2(H2 O)'
_chemical_formula_sum            'C78 H76 N16 Ni3 O18'
_chemical_formula_weight         1701.67
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-28 deposited with the CCDC.	2021-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                103.4100(10)
_cell_angle_beta                 108.6770(10)
_cell_angle_gamma                95.7550(10)
_cell_formula_units_Z            1
_cell_length_a                   11.0003(6)
_cell_length_b                   12.7408(7)
_cell_length_c                   15.3439(8)
_cell_measurement_reflns_used    8142
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      30.672
_cell_measurement_theta_min      2.345
_cell_volume                     1945.82(18)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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_temperature      293.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.793
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0106
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.793
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12865
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.793
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.837
_diffrn_reflns_theta_min         2.634
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0434 before and 0.0212 after correction. The Ratio of minimum to maximum transmission is 0.8385. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       block
_exptl_crystal_F_000             884
_refine_diff_density_max         1.184
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         9695
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.221
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0470P)^2^+2.3386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1408
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8515
_reflns_number_total             9695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01702g2.cif
_cod_data_source_block           yd0686_0m
_cod_depositor_comments
'Adding full bibliography for 7242112--7242117.cif.'
_cod_database_code               7242114
_shelx_shelxl_version_number     2018/3
_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 O(H,H) groups
2. Restrained distances
 C13-C14 = C9-C10 = C11-C12
 1.4 with sigma of 0.02
3. Others
 Fixed Sof: O5(0.5) O10(0.5) C8(0.5) H8C(0.5) H8D(0.5) C9(0.5) C14(0.5)
 H14(0.5) C13(0.5) H13(0.5) C12(0.5) H12(0.5) C11(0.5) H11(0.5) C10(0.5)
 C43(0.5) H43A(0.5) H43B(0.5) C45(0.5) C46(0.5)
4.a Free rotating group:
 O9(H9A,H9B)
4.b Rotating group:
 O6(H6A,H6B), O8(H8A,H8B)
4.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C5(H5A,H5B), C8(H8C,H8D), C43(H43A,H43B)
4.d Aromatic/amide H refined with riding coordinates:
 C14(H14), C13(H13), C12(H12), C11(H11), C15(H15), C17(H17), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
;
_shelx_res_checksum              3882
_shelx_hkl_checksum              32660
_olex2_submission_special_instructions 'No special instructions were received'