Indole-based mono- and poly-nuclear acyclic chelating systems: syntheses and selected transition metal complexes
Paul K. Bowyer; David StC. Black; Donald C. Craig; A. David Rae; Anthony C. Willis; J. Chem. Soc., Dalton Trans.  (2001) 1948–1958; doi:10.1039/b101350p

data_7010627
_publ_section_title
;
 Indole-based mono- and poly-nuclear acyclic chelating systems:
 syntheses and selected transition metal complexes
;
_journal_issue                   13
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1948
_journal_page_last               1958
_journal_paper_doi               10.1039/b101350p
_journal_year                    2001
_chemical_formula_moiety         'C80 H60 Cl4 N8 Ni2 O8, 7(C3 H7 N O) '
_chemical_formula_sum            'C101 H109 Cl4 N15 Ni2 O15'
_chemical_formula_weight         2032.28
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             1999-12-13
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
1997  data collected and structure solved in xtal/texsan
1999  solution improved with use of RAELS
report and rough cif from adr to acw
2000-03-31 - Report and cif on pxb15 compiled by Anthony C. Willis
2000-04-03 - sent to checkcif.  Reply gives anticipated alerts
2001-04-09 - response to referees' reports
;
_cell_angle_alpha                70.36(6)
_cell_angle_beta                 71.35(6)
_cell_angle_gamma                85.15(7)
_cell_formula_units_Z            1
_cell_length_a                   12.952(12)
_cell_length_b                   14.602(12)
_cell_length_c                   15.286(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    273.2
_cell_measurement_theta_max      12.69
_cell_measurement_theta_min      9.64
_cell_volume                     2579(4)
_computing_cell_refinement       xtal_LATCON
_computing_data_collection
;
Philips PW1100/20 software 1976
;
_computing_data_reduction        xtal_DIFDAT_ADDREF
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  RAELS96
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1993)
;
_diffrn_ambient_temperature      273.2
_diffrn_measurement_device_type  'Philips PW1100/20'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_av_sigmaI/netI    0.080
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9527
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        5
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1064.00
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.296
_refine_ls_goodness_of_fit_ref   1.530
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4299
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.152
_refine_ls_R_factor_gt           0.074
_refine_ls_shift/su_max          0.3
_refine_ls_shift/su_mean         0.1
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + (0.05Fo)^2^] '
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.121
_refine_ls_wR_factor_ref         0.101
_reflns_number_gt                4299
_reflns_number_total             9135
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            b101350p.txt
_cod_data_source_block           9a
_cod_original_sg_symbol_H-M      'P -1       '
_cod_database_code               7010627