Low-temperature phase of bis(2-methoxycarbonyl-2-methylpropyl) 2,5-diisopropylidene-3,4-bis(2-methoxycarbonyl-2-methylpropoxycarbonyl)hex-3-enedioate, a crystal structure with six independent pseudo-related molecules
Bats, Jan W.; Rivas Nass, Andreas; Hashmi, A. Stephen K.; Acta Crystallographica Section C 55 (1999) 1183–1186; doi:10.1107/S0108270199003078

data_2008729
_publ_section_title
;Low-temperature phase of bis(2-methoxycarbonyl-2-methylpropyl)
 2,5-diisopropylidene-3,4-bis(2-methoxycarbonyl-2-methylpropoxycarbonyl)hex-3-enedioate,
 a crystal structure with six independent pseudo-related molecules
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1183
_journal_page_last               1186
_journal_paper_doi               10.1107/S0108270199003078
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C38 H56 O16'
_chemical_formula_weight         768.83
_chemical_melting_point          337
_chemical_name_systematic
;
2,5-Diisopropylidene-3,4-bis-(2-methoxycarbonyl-2-methylpropoxycarbonyl)-hex-
3-enedioic acid bis(2-methoxycarbonyl-2-methylpropyl)ester
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 102.696(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   26.280(4)
_cell_length_b                   26.285(3)
_cell_length_c                   18.449(2)
_cell_measurement_reflns_used    235
_cell_measurement_temperature    136(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     12432(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    XP_in_SHELXTL_(Sheldrick,_1996)
_computing_publication_material  CIF_in_SHELXL-97_(Sheldrick,_1997)
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1996)'
_diffrn_ambient_temperature      136(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'Siemens Smart'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1277
_diffrn_reflns_av_sigmaI/netI    0.1946
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            207489
_diffrn_reflns_theta_full        30.36
_diffrn_reflns_theta_max         30.36
_diffrn_reflns_theta_min         1.37
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  540
_diffrn_standards_number         775
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  1.0
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             4944
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.281
_refine_ls_abs_structure_details 'Flack  (1983)'
_refine_ls_abs_structure_Flack   -0.1(7)
_refine_ls_extinction_coef       0.00039(3)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2966
_refine_ls_number_reflns         62820
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.2369
_refine_ls_R_factor_gt           0.0780
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1570
_reflns_number_gt                26218
_reflns_number_total             62820
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1272.cif
_cod_data_source_block           pc
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '337 K' was changed to '337' - the
value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '337 K' was changed to '337' - the
value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               2008729
_cod_database_fobs_code          2008729