Nickel(II) Bis(<i>d</i>-campholyl-<i>l</i>-campholylmethanate)
Ficker, R.; Hiller, W.; Ossig, A.; Schurig, V.; Acta Crystallographica Section C 52 (1996) 543–545; doi:10.1107/S0108270195010663

data_2004604
_publ_section_title
;
 Nickel(II) Bis(<i>d</i>-campholyl-<i>l</i>-campholylmethanate)
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              543
_journal_page_last               545
_journal_paper_doi               10.1107/S0108270195010663
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[Ni1 (C21 H35 O2)2]'
_chemical_formula_moiety         'C42 H70 Ni O4'
_chemical_formula_sum            'C42 H70 Ni O4'
_chemical_formula_weight         697.69
_chemical_name_common            Nickel(II)-bis-[(d,l)-dicampholylmethanat]
_chemical_name_systematic
;
Nickel(II)-bis[1-((+)-(1'R,3'S)-1',2',2',3'-tetramethyl-cyclopent-1'yl)-
3-((-)-(1'S,3'R)-1',2',2',3'-tetramethyl-cyclopent-1'yl)-propan-1,3-
dionate]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           'from SHELXL-93'
_cell_angle_alpha                114.805(9)
_cell_angle_beta                 98.699(9)
_cell_angle_gamma                100.923(9)
_cell_formula_units_Z            1
_cell_length_a                   7.3319(8)
_cell_length_b                   12.3885(9)
_cell_length_c                   12.8313(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      38
_cell_measurement_theta_min      16
_cell_volume                     1003.38(19)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'CADHKL4 in CADSHEL (Kopf & Ruebcke, 1993)'
_computing_molecular_graphics    'SHELXTL/PC (Siemens, 1990)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  '0.016 (F)'
_diffrn_reflns_av_sigmaI/netI    0.0140
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3715
_diffrn_reflns_theta_max         65
_diffrn_reflns_theta_min         4
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.201
_exptl_absorpt_correction_type   'empirical (DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       needles
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         .395
_refine_diff_density_min         -.274
_refine_ls_extinction_coef       0.0120(10)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   1.119
_refine_ls_goodness_of_fit_obs   1.126
_refine_ls_hydrogen_treatment
;
H(2) refined freely, other H atoms refined as riding model
(SHELXL93; Sheldrick, 1993)
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         1432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_restrained_S_obs      1.126
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_obs          0.0446
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.1130P)^2^ + 1.6245P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1204
_refine_ls_wR_factor_obs         0.1163
_reflns_number_observed          1432
_reflns_number_total             3419
_reflns_observed_criterion       >4sigma(F)
_cod_data_source_file            fg1065.cif
_cod_data_source_block           ossig
_cod_original_cell_volume        1003.37(2)
_cod_original_formula_sum        'C42 H70 Ni1 O4'
_cod_database_code               2004604