Stereospecific solid-state cyclodimerization of bis(trans-2-butenoato)calcium and triaquabis(trans-2-butenoato)magnesium
Hickey, Magali B.; Schlam, Roxana F.; Guo, Chengyun; Cho, Tae H.; Snider, Barry B.; Foxman, Bruce M.; CrystEngComm 13 (2011) 3146–; doi:10.1039/c0ce00535e

data_7205653
_publ_section_title
;
 Stereospecific solid-state cyclodimerization of
 bis(trans-2-butenoato)calcium and
 triaquabis(trans-2-butenoato)magnesium
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              3146
_journal_paper_doi               10.1039/c0ce00535e
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C4 H5.00 Ca0.50 O2'
_chemical_formula_sum            'C4 H5 Ca0.5 O2'
_chemical_formula_weight         105.12
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-06-11
_audit_creation_method           CRYSTALS_ver_14.01
_cell_angle_alpha                90
_cell_angle_beta                 100.415(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.536(3)
_cell_length_b                   5.2295(5)
_cell_length_c                   6.4483(8)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    294
_cell_measurement_theta_max      28
_cell_measurement_theta_min      21
_cell_volume                     482.10(13)
_computing_cell_refinement       'CAD4 EXPRESS, (Straver, 1992)'
_computing_data_collection       'CAD4 EXPRESS, (Straver, 1992)'
_computing_data_reduction        'RC93 (Watkin et al., 1994)'
_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      294
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       Serial
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1587
_diffrn_reflns_theta_full        29.834
_diffrn_reflns_theta_max         30.443
_diffrn_reflns_theta_min         3.896
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             220
_exptl_crystal_size_max          0.684
_exptl_crystal_size_mid          0.592
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.32
_refine_ls_extinction_coef       32(11)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0087
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1246
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.0008145
_refine_ls_shift/su_mean         0.0005897
_refine_ls_structure_factor_coef F
_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:
2.22 0.977 1.71
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0594
_refine_ls_wR_factor_gt          0.0420
_refine_ls_wR_factor_ref         0.0420
_reflns_limit_h_max              20
_reflns_limit_h_min              0
_reflns_limit_k_max              7
_reflns_limit_k_min              0
_reflns_limit_l_max              8
_reflns_limit_l_min              -9
_reflns_number_gt                1246
_reflns_number_total             1462
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0333
_oxford_refine_ls_scale          2.224(7)
_oxford_reflns_number_all        1462
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title CACROPYR
_cod_data_source_file            c0ce00535e.txt
_cod_data_source_block           compound_4
_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_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

data name '_diffrn_measurement_device-type' was replaced with
'_diffrn_measurement_device_type' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        482.11(13)
_cod_original_sg_symbol_H-M      'P 1 2/c 1 '
_cod_original_formula_sum        'C4 H5.00 Ca0.50 O2'
_cod_database_code               7205653