Synthesis, characterisation and redox properties of anti-bimetallic permethylpentalene complexes.
Binding, Samantha C.; Green, Jennifer C.; Turner, Zoë R; Buffet, Jean-Charles; O'Hare, Dermot; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4263–4273; doi:10.1039/c8dt05054f

data_7049184
_publ_section_title
;
 Synthesis, characterisation and redox properties of anti-bimetallic
 permethylpentalene complexes.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4263
_journal_page_last               4273
_journal_paper_doi               10.1039/c8dt05054f
_journal_volume                  48
_journal_year                    2019
_chemical_compound_source        SYN
_chemical_formula_moiety         'C24 H28 Ni2'
_chemical_formula_sum            'C24 H28 Ni2'
_chemical_formula_weight         433.91
_chemical_melting_point          ?
_chemical_name_systematic        bis(cyclopentadienylnickel)pentalenyl
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-06-02
_audit_creation_method           CRYSTALS_ver_14.43
_audit_update_record
;
2018-12-20 deposited with the CCDC.    2019-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                68.600(3)
_cell_angle_beta                 87.710(3)
_cell_angle_gamma                62.426(4)
_cell_formula_units_Z            1
_cell_length_a                   7.6274(4)
_cell_length_b                   8.2173(4)
_cell_length_c                   9.6561(7)
_cell_measurement_reflns_used    1880
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     493.35(6)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6788
_diffrn_reflns_theta_full        25.039
_diffrn_reflns_theta_max         27.516
_diffrn_reflns_theta_min         5.246
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.912
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'brown black'
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             228
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.87
_refine_diff_density_min         -0.64
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8807
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2245
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.0007542
_refine_ls_shift/su_mean         0.0000170
_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: 
 101. 162. 98.0 40.8 9.70 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1017
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1017
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              10
_reflns_limit_k_min              -9
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                2099
_reflns_number_total             2245
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.66
_oxford_diffrn_Wilson_scale      0.33
_oxford_refine_ls_r_factor_ref   0.0441
_oxford_refine_ls_scale          1.711(14)
_oxford_reflns_number_all        2245
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '044scb14 At 18:16 on 2/ 6'
_cod_data_source_file            c8dt05054f2.cif
_cod_data_source_block           5-044scb14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

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

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7049180--7049184.cif.
;
_cod_original_cell_volume        493.35(5)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7049184
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
SUMFIX ELEMENT SCALES 
RIDE C   (   5,X'S) H   (  51,X'S) H   (  53,X'S) H   (  52,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  63,X'S) H   (  62,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) H   (  73,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;