A Triad of Bis(orthometalated) d8-Complexes Containing Four-Membered Rings
Bennett, Martin A.; Bhargava, Suresh K.; Keniry, Max A.; Privér, Steven H.; Simmonds, Peta M.; Wagler, Jörg; Willis, Anthony C.; Organometallics 27 (2008) 5361–; doi:10.1021/om8004806

data_4071944
_publ_section_title
;
 A Triad of Bis(orthometalated) d8-Complexes Containing Four-Membered
 Rings
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5361
_journal_paper_doi               10.1021/om8004806
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source
;
from RMITU
;
_chemical_formula_moiety         'C37 H20 F8 O3 P2, 0.572(H2 O)'
_chemical_formula_sum            'C37 H21.144 F8 O3.572 P2'
_chemical_formula_weight         736.77
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-03-19
_audit_creation_method           CRYSTALS_ver_12.18
_audit_update_record
;
2008-03-19 - Report on C37 H21.144 F8 O3.572 P2
              by   Anthony C. Willis
              for  Steven Priver and Martin Bennett

2008-03-19 - passes checkcif tests with minor warnings
;
_cell_angle_alpha                90
_cell_angle_beta                 98.1043(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6431(1)
_cell_length_b                   12.5819(1)
_cell_length_c                   26.2617(3)
_cell_measurement_reflns_used    49036
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     3154.47(5)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material  'CRYSTALS (Watkin et al 2003)'
_computing_structure_refinement  'CRYSTALS (Watkin et al 2003)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            62122
_diffrn_reflns_theta_full        27.530
_diffrn_reflns_theta_max         27.530
_diffrn_reflns_theta_min         2.678
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1494.82
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9857
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         7256
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.004654
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
  Method, part 1, Chebychev polynomial,
(Watkin, 1994, Prince, 1982)
  [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
  where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
  Method = Robust Weighting (Prince, 1982)
  W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
  A~i~ are:
  20.5 32.3 18.0 6.48 0.909
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1054
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.1054
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                4515
_reflns_number_total             7256
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.58
_oxford_diffrn_Wilson_scale      9.43
_oxford_refine_ls_scale          0.2774(2)
_oxford_structure_analysis_title '3181618 ben0801'
_cod_data_source_file            om8004806_si_001.cif
_cod_data_source_block           ben0801
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4071944