#------------------------------------------------------------------------------
#$Date: 2017-01-17 07:21:32 +0100 (mar 17 de ene de 2017) $
#$Revision: 190580 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/74/7227443.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7227443
loop_
_publ_author_name
'Al-Khafaji, Yahya F.'
'Elsegood, Mark R. J.'
'Frese, Josef W. A.'
'Redshaw, Carl'
_publ_section_title
;
 Ring opening polymerization of lactides and lactones by multimetallic
 alkyl zinc complexes derived from the acids Ph2C(X)CO2H (X = OH, NH2)
;
_journal_issue                   8
_journal_name_full               'RSC Adv.'
_journal_page_first              4510
_journal_paper_doi               10.1039/C6RA26746G
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C4 H6 Cl2 N2 Zn'
_chemical_formula_sum            'C4 H6 Cl2 N2 Zn'
_chemical_formula_weight         218.38
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-11-11 deposited with the CCDC.
2016-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7113(11)
_cell_length_b                   9.9296(8)
_cell_length_c                   6.5812(6)
_cell_measurement_reflns_used    4598
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.39
_cell_measurement_theta_min      3.21
_cell_volume                     830.67(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9419
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.711
_diffrn_reflns_theta_min         3.205
_exptl_absorpt_coefficient_mu    3.518
_exptl_absorpt_correction_T_max  0.401
_exptl_absorpt_correction_T_min  0.154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2004/1, Sheldrick, G.M., (2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.750
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.260
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0047(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         1440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0326P)²+0.1445P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0535
_refine_ls_wR_factor_ref         0.0550
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1284
_reflns_number_total             1440
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ra26746g2.cif
_cod_data_source_block           ZnCl2_NCMe_2
_cod_database_code               7227443
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.178
_shelx_estimated_absorpt_t_max   0.462
_shelx_res_file
; 
  
    cr263.res created by SHELXL-2014/7 
  
  
TITL cr263 in Pnma 
CELL 0.71073  12.7113   9.9296   6.5812  90.000  90.000  90.000 
ZERR    4.00   0.0011   0.0008   0.0006   0.000   0.000   0.000 
LATT  1 
SYMM 0.5-X, -Y, 0.5+Z 
SYMM -X, 0.5+Y, -Z 
SYMM 0.5+X, 0.5-Y, 0.5-Z 
SFAC C H N CL ZN 
UNIT 16 24 8 8 4 
TEMP -123 
SIZE 0.26 0.36 0.75 
  
ACTA 
CONF 
WPDB -1 
  
OMIT 4 0 0 
L.S. 8 
BOND $H 
LIST 4 
FMAP 2 
PLAN 10 
  
WGHT    0.032600    0.144500 
EXTI    0.004735 
FVAR       0.60868 
ZN1   5   -0.004422    0.750000    0.027102    10.50000    0.01889    0.02056 = 
         0.01710    0.00000    0.00129    0.00000 
CL1   4    0.167704    0.750000    0.068818    10.50000    0.01905    0.03094 = 
         0.02975    0.00000    0.00003    0.00000 
CL2   4   -0.072856    0.750000   -0.280452    10.50000    0.03205    0.03299 = 
         0.02072    0.00000   -0.00595    0.00000 
N1    3   -0.069479    0.598176    0.194139    11.00000    0.02706    0.02532 = 
         0.02483    0.00163    0.00159   -0.00176 
C1    1   -0.113095    0.529713    0.302858    11.00000    0.02191    0.02184 = 
         0.02192   -0.00061    0.00024    0.00067 
C2    1   -0.170164    0.443298    0.441689    11.00000    0.04025    0.02676 = 
         0.03227    0.00646    0.01205   -0.00490 
AFIX 137 
H2A   2   -0.203198    0.498282    0.547618    11.00000   -1.50000 
H2B   2   -0.121346    0.379217    0.504425    11.00000   -1.50000 
H2C   2   -0.224565    0.393918    0.366972    11.00000   -1.50000 
AFIX   0 
HKLF 4 
  
REM  cr263 in Pnma 
REM R1 =  0.0199 for    1284 Fo > 4sig(Fo)  and  0.0236 for all    1440 data 
REM     48 parameters refined using      0 restraints 
  
END 
  
WGHT      0.0326      0.1445 
  
REM Highest difference peak  0.356,  deepest hole -0.304,  1-sigma level  0.066 
Q1    1   0.0570  0.7500  0.0250  10.50000  0.05    0.36 
Q2    1  -0.0034  0.6909 -0.0432  11.00000  0.05    0.35 
Q3    1  -0.0057  0.6897  0.1030  11.00000  0.05    0.34 
Q4    1  -0.1393  0.4686  0.3753  11.00000  0.05    0.33 
Q5    1  -0.0655  0.7500  0.0259  10.50000  0.05    0.30 
Q6    1  -0.2424  0.5070  0.4542  11.00000  0.05    0.30 
Q7    1   0.1754  0.6791  0.1274  11.00000  0.05    0.29 
Q8    1  -0.2524  0.4649  0.4505  11.00000  0.05    0.29 
Q9    1  -0.0801  0.6967 -0.2049  11.00000  0.05    0.26 
Q10   1  -0.0613  0.5487  0.2836  11.00000  0.05    0.25 
;
_shelx_res_checksum              76215
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Zn1 Zn -0.00442(2) 0.7500 0.02710(3) 0.01885(8) Uani 1 2 d S T P
Cl1 Cl 0.16770(3) 0.7500 0.06882(7) 0.02658(11) Uani 1 2 d S T P
Cl2 Cl -0.07286(3) 0.7500 -0.28045(7) 0.02859(11) Uani 1 2 d S T P
N1 N -0.06948(8) 0.59818(11) 0.19414(16) 0.0257(2) Uani 1 1 d . . .
C1 C -0.11310(9) 0.52971(12) 0.30286(18) 0.0219(2) Uani 1 1 d . . .
C2 C -0.17016(12) 0.44330(15) 0.4417(2) 0.0331(3) Uani 1 1 d . . .
H2A H -0.2032 0.4983 0.5476 0.050 Uiso 1 1 calc R U .
H2B H -0.1213 0.3792 0.5044 0.050 Uiso 1 1 calc R U .
H2C H -0.2246 0.3939 0.3670 0.050 Uiso 1 1 calc R U .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.01889(11) 0.02056(12) 0.01710(12) 0.000 0.00129(6) 0.000
Cl1 0.01905(19) 0.0309(2) 0.0298(2) 0.000 0.00003(15) 0.000
Cl2 0.0320(2) 0.0330(2) 0.02072(18) 0.000 -0.00595(16) 0.000
N1 0.0271(5) 0.0253(5) 0.0248(5) 0.0016(4) 0.0016(4) -0.0018(4)
C1 0.0219(5) 0.0218(5) 0.0219(5) -0.0006(4) 0.0002(4) 0.0007(4)
C2 0.0403(8) 0.0268(6) 0.0323(7) 0.0065(5) 0.0120(6) -0.0049(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Zn1 N1 95.24(6) . 7_575
N1 Zn1 Cl2 109.57(3) . .
N1 Zn1 Cl2 109.57(3) 7_575 .
N1 Zn1 Cl1 109.57(3) . .
N1 Zn1 Cl1 109.57(3) 7_575 .
Cl2 Zn1 Cl1 120.408(19) . .
C1 N1 Zn1 169.27(10) . .
N1 C1 C2 179.21(14) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 N1 2.0408(11) .
Zn1 N1 2.0409(11) 7_575
Zn1 Cl2 2.2031(5) .
Zn1 Cl1 2.2051(5) .
N1 C1 1.1320(15) .
C1 C2 1.4482(17) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
