Hydrolytically active tetranuclear [NiII2]2 complexes: synthesis, structure, spectroscopy and phosphoester hydrolysis
Giri, Gopal C.; Patra, Ayan; Vijaykumar, Gonela; Carrella, Luca; Bera, Manindranath; RSC Advances 5 (2015) 99270–; doi:10.1039/C5RA16555E

data_7235969
_publ_section_title
;
 Hydrolytically active tetranuclear [NiII2]2 complexes: synthesis,
 structure, spectroscopy and phosphoester hydrolysis
;
_journal_issue                   120
_journal_name_full               'RSC Advances'
_journal_page_first              99270
_journal_paper_doi               10.1039/C5RA16555E
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C46 H62 N4 Ni4 O18, 2(Br1), 4(C H4 O), 3(O)'
_chemical_formula_sum            'C50 H84 Br2 N4 Ni4 O25'
_chemical_formula_weight         1535.87
_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
_audit_creation_date             2015-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-11-09 deposited with the CCDC.
2015-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                109.907(2)
_cell_angle_beta                 93.565(3)
_cell_angle_gamma                107.606(3)
_cell_formula_units_Z            1
_cell_length_a                   10.7231(14)
_cell_length_b                   11.7791(16)
_cell_length_c                   13.9580(19)
_cell_measurement_temperature    273(2)
_cell_volume                     1553.0(4)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97/(Altomare, 1997)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'BRUKER SMART APEX CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA-PHI SCAN'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21101
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.783
_diffrn_reflns_theta_min         1.959
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       Plate
_exptl_crystal_F_000             794
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   0.664
_exptl_transmission_factor_min   0.483
_refine_diff_density_max         1.015
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         5331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0475P)^2^+3.3701P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1034
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4388
_reflns_number_total             5331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra16555e2.cif
_cod_data_source_block           complex
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               7235969
_shelxl_version_number           2012-9
_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, All O(H) groups, All O(H,H) groups
2. Others
 Sof(Br1B)=1-FVAR(1)
 Sof(Br1A)=FVAR(1)
 Fixed Sof: O13(0.55) O13B(0.25) O13C(0.2) O1WA(0.16667) O1WB(0.16667)
 O1WC(0.16666)
3.a Riding coordinates:
 O9(H9A,H9B), O10(H10), O11(H11), O12(H12A,H12B)
3.b Ternary CH refined with riding coordinates:
 C4(H4)
3.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C12(H12C,H12D), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B)
3.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10A), C11(H11A), C20(H20), C21(H21), C22(H22), C23(H23)
3.e Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
3.f Idealised tetrahedral OH refined as rotating group:
 O7(H7), O8(H8A)
;
_shelx_res_checksum              53892
_olex2_submission_special_instructions 'No special instructions were received'